[ CAS No. 442908-10-3 ] {[proInfo.proName]}

Name: 442908-10-3|3-(4-Amino-3-methylbenzyl)-7-(furan-2-yl)-3H-[1,2,3]triazolo[4,5-d]pyrimidin-5-amine|98%
Brand: Ambeed
SKU: A155723
Price: 13.0 USD
Availability: InStock
Rating: 90 (32 reviews)

,{[proInfo.pro_purity]}

Cat. No.: {[proInfo.prAm]}

2D 3D

Structure of 442908-10-3 * Storage: {[proInfo.prStorage]}

Cart0 Add to My Favorites Add to My Favorites Bulk Inquiry Inquiry Add To Cart

Search after Editing

* Storage: {[proInfo.prStorage]}

For Research Only 110K+ Compounds Competitive Price 1-2 Day Shipping

Quality Control of [ 442908-10-3 ]

COA NMR CNMR HPLC LC-MS

Related Doc. of [ 442908-10-3 ]

SDS Specification

Alternatived Products of [ 442908-10-3 ]

Product Details of [ 442908-10-3 ]

CAS No. :	442908-10-3	MDL No. :	MFCD12024697
Formula :	C₁₆H₁₅N₇O	Boiling Point :	-
Linear Structure Formula :	-	InChI Key :	HQSBCDPYXDGTCL-UHFFFAOYSA-N
M.W :	321.34	Pubchem ID :	21874557
Synonyms :	BIIB-014;CEB-4520;VER-ADO-49;VER-A00049;VER-A00-11;VER-11135;V-2006

Calculated chemistry of [ 442908-10-3 ]

Physicochemical Properties

Num. heavy atoms :	24
Num. arom. heavy atoms :	20
Fraction Csp3 :	0.12
Num. rotatable bonds :	3
Num. H-bond acceptors :	5.0
Num. H-bond donors :	2.0
Molar Refractivity :	90.34
TPSA :	121.67 Å²

Pharmacokinetics

GI absorption :	High
BBB permeant :	No
P-gp substrate :	Yes
CYP1A2 inhibitor :	Yes
CYP2C19 inhibitor :	No
CYP2C9 inhibitor :	No
CYP2D6 inhibitor :	No
CYP3A4 inhibitor :	Yes
Log Kp (skin permeation) :	-7.25 cm/s

Lipophilicity

Log Po/w (iLOGP) :	2.33
Log Po/w (XLOGP3) :	1.42
Log Po/w (WLOGP) :	2.02
Log Po/w (MLOGP) :	1.14
Log Po/w (SILICOS-IT) :	1.16
Consensus Log Po/w :	1.61

Druglikeness

Lipinski :	0.0
Ghose :	None
Veber :	0.0
Egan :	0.0
Muegge :	0.0
Bioavailability Score :	0.55

Water Solubility

Log S (ESOL) :	-3.15
Solubility :	0.23 mg/ml ; 0.000715 mol/l
Class :	Soluble
Log S (Ali) :	-3.58
Solubility :	0.0846 mg/ml ; 0.000263 mol/l
Class :	Soluble
Log S (SILICOS-IT) :	-5.27
Solubility :	0.00173 mg/ml ; 0.00000538 mol/l
Class :	Moderately soluble

Medicinal Chemistry

PAINS :	0.0 alert
Brenk :	1.0 alert
Leadlikeness :	0.0
Synthetic accessibility :	3.14

Safety of [ 442908-10-3 ]

Signal Word:	Warning	Class:	N/A
Precautionary Statements:	P261-P305+P351+P338	UN#:	N/A
Hazard Statements:	H302-H315-H319-H335	Packing Group:	N/A
GHS Pictogram:

Application In Synthesis of [ 442908-10-3 ]

* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.

Upstream synthesis route of [ 442908-10-3 ]
Downstream synthetic route of [ 442908-10-3 ]

[ 442908-10-3 ] Synthesis Path-Upstream 1~2

1
[ 442908-07-8 ]
[ 442908-10-3 ]

Yield	Reaction Conditions	Operation in experiment
92%	With formic acid; triethylamine In tetrahydrofuran at 70℃; for 5 h;	Example 4: Preparation of3-(4-amino-3-methylbenzyl)-7-(furan-2-yl)-3H- [l,2,3]triazolo[4,5-d]pyrimidin-5-amine (1) A 250 mL 2-necked round-bottomed flask was charged with 7-(furan-2-yl)-3-(3- methyl-4-nitrobenzyl)-3H-[l,2,3]triazolo[4,5-d]pyrimidin-5-amine (3.0 g, 8.5 mmol) and 5percent Pd/C catalyst (0.46 g, 0.073 mmol) under a nitrogen atmosphere. Next, THF (72 mL) and triethylamine (9.0 mL, 65 mmol) were added via syringe and the resulting mixture was stirred to obtain slurry. Formic acid (2.3 mL, 46.03 mmol) was then added all at once, and the mixture was heated with a bath set to a temperature of 70 ⁰C. After 5 hours the reaction was cooled to 25 ⁰C. Water (60 mL) was added, and concentrated hydrochloric acid was added dropwise to dissolve the product. The solution was filtered through Celite 545 to remove the catalyst, and the filter cake was washed with additional water (2 X 5 mL). To the yellowish filtrate was added 50percent sodium hydroxide in water to precipitate the product. The mixture was stirred for an additional hour before isolation by filtration. The filter cake was washed with water (10 mL) then methanol (10 mL). The product was dried under vacuum to constant weight to yield 2.79 g (92percent) of 3-(4-amino- 3-methylbenzyl)-7-(furan-2-yl)-3H-[l,2,3]triazolo[4,5-d]pyrimidin-5-amine.

Reference： [1] Patent: WO2008/86201, 2008, A1, . Location in patent: Page/Page column 21
[2] Journal of Medicinal Chemistry, 2009, vol. 52, # 1, p. 33 - 47

2
[ 442906-78-7 ]
[ 141281-38-1 ]
[ 442908-10-3 ]

Reference： [1] Journal of Medicinal Chemistry, 2009, vol. 52, # 1, p. 33 - 47

[ 442908-10-3 ] Synthesis Path-Downstream 1~10

Yield	Reaction Conditions	Operation in experiment
	In ethanol; water; dimethyl sulfoxide; at 20 - 83℃; for 6.0h;Purification / work up;	Alternatively, a glass lined 1000 L reactor was charged with 58.3 kg wet, crude compound 1. After purging the reactor with nitrogen, the reactor was charged with 289 kg DMSO, and the mixture was heated to 77 - 83 0C. A solution was obtained, to which 210L of ethanol 96% was added in 75 min at 77 - 83 0C, whereby crystallization started.Then, 105 L of purified water were added in 45 min at 77 - 83 0C. After the addition of water was complete, the mixture was cooled to 20 - 25 0C in 3 hours and stirred at this temperature for 1 hour. The product was filtered, and the filter cake was washed three times with 84 L of ethanol 96% each, the first two washings being performed with stirring. Finally, the product, wet, pure compound 1, was discharged.For XRPD, the relative intensities of the peaks can vary depending on, for example, the sample preparation technique, the sample mounting procedure, and the particular instrument employed. Instrument variation and other factors can also affect the measured values of 2Theta. Accordingly, XRPD peak assignments can vary by plus or minus0.2 in 2Theta.For DSC, observed temperatures will depend on the rate of temperature change as well as sample preparation technique and the particular instrument employed. Thus, the values reported for DSC thermograms can vary by plus or minus about 4 0C. FIG. IA shows an XRPD trace of crystal form A. The XRPD pattern of crystal form A is characterized by peaks at 2Theta of 7.20, 8.14, 10.26, 13.00, 14.23, 15.10,17.75, 18.20, 19.31, 20.41, 22.15, 23.36, 24.19, 25.55, 26.39, 27.26, and 28.62. FIG. IB shows a DSC thermogram for crystal form A. Crystal form A shows a minimum in DSC thermograms (i.e., melting point) at about 243 0C - 246 0C, with a DeltaHf of between 154.5 J/g and 165.8 J/g. DSC analysis before and after micronisation showed no significant difference in the heat of fusion, confirming that micronisation did not adversely affect crystalline quality.FIG. 1C shows a TGA trace for crystal form A. TGA revealed that form A was substantially free of solvent; weight loss from ambient temperature to 220 0C varied between < 0.1 %w/w to 1.2 %w/w. TGA analysis before and after micronisation showed that micronised material contained less unbound and less trapped solvent than the pre- micronised material.
	In butan-1-ol; at 20 - 50℃; for 144.0h;Purification / work up;	Example 11: Recrystallization From Various Solvents500muL of each of 24 solvents were added to 50 mg +/- 5 mg of form A, to produce a saturated solution. If complete dissolution was achieved, additional material was added until an excess of solid was present.The vials were capped and placed in a shaking incubator which cycled between ambient temperature and 50 0C, changing every 12 hours. Shaking was continued for 4 days. Inspection of the vials showed that the majority of the 1,1,1,3,3,3- hexafluoropropan-2-ol had evaporated, so an additional 500 muL was added. Inspection after another 2 days showed that this vial now contained only a solution, so additional solid (~30mg) was added.A sample of each slurry was transferred to a glass slide, partially dried either by evaporation or by wicker filtration of any excess solvent and examined by XRPD. Recrystallization from l,l,l,3,3,3-hexafluoro-propan-2-ol afforded crystal form G (see above). Under these conditions, recrystallization from acetone, acetonitrile, THF, DMA, DCM, cyclohexane, heptane, n-butanol, DMF, 1,4-dioxane, ethyl acetate, ethanol, butyl acetate, /-propyl acetate, MEK, methanol, MIBK, propan-1-ol, propan-2-ol, t-BME, toluene, water, or NMP afforded crystal form A.
	In dichloromethane; at 20 - 50℃; for 144.0h;Purification / work up;	Example 11: Recrystallization From Various Solvents500muL of each of 24 solvents were added to 50 mg +/- 5 mg of form A, to produce a saturated solution. If complete dissolution was achieved, additional material was added until an excess of solid was present.The vials were capped and placed in a shaking incubator which cycled between ambient temperature and 50 0C, changing every 12 hours. Shaking was continued for 4 days. Inspection of the vials showed that the majority of the 1,1,1,3,3,3- hexafluoropropan-2-ol had evaporated, so an additional 500 muL was added. Inspection after another 2 days showed that this vial now contained only a solution, so additional solid (~30mg) was added.A sample of each slurry was transferred to a glass slide, partially dried either by evaporation or by wicker filtration of any excess solvent and examined by XRPD. Recrystallization from l,l,l,3,3,3-hexafluoro-propan-2-ol afforded crystal form G (see above). Under these conditions, recrystallization from acetone, acetonitrile, THF, DMA, DCM, cyclohexane, heptane, n-butanol, DMF, 1,4-dioxane, ethyl acetate, ethanol, butyl acetate, /-propyl acetate, MEK, methanol, MIBK, propan-1-ol, propan-2-ol, t-BME, toluene, water, or NMP afforded crystal form A.

	In ethyl acetate; at 20 - 50℃; for 144.0h;Purification / work up;	Example 11: Recrystallization From Various Solvents500muL of each of 24 solvents were added to 50 mg +/- 5 mg of form A, to produce a saturated solution. If complete dissolution was achieved, additional material was added until an excess of solid was present.The vials were capped and placed in a shaking incubator which cycled between ambient temperature and 50 0C, changing every 12 hours. Shaking was continued for 4 days. Inspection of the vials showed that the majority of the 1,1,1,3,3,3- hexafluoropropan-2-ol had evaporated, so an additional 500 muL was added. Inspection after another 2 days showed that this vial now contained only a solution, so additional solid (~30mg) was added.A sample of each slurry was transferred to a glass slide, partially dried either by evaporation or by wicker filtration of any excess solvent and examined by XRPD. Recrystallization from l,l,l,3,3,3-hexafluoro-propan-2-ol afforded crystal form G (see above). Under these conditions, recrystallization from acetone, acetonitrile, THF, DMA, DCM, cyclohexane, heptane, n-butanol, DMF, 1,4-dioxane, ethyl acetate, ethanol, butyl acetate, /-propyl acetate, MEK, methanol, MIBK, propan-1-ol, propan-2-ol, t-BME, toluene, water, or NMP afforded crystal form A.
	In isopropyl alcohol; at 20 - 50℃; for 144.0h;Purification / work up;	Example 11: Recrystallization From Various Solvents500muL of each of 24 solvents were added to 50 mg +/- 5 mg of form A, to produce a saturated solution. If complete dissolution was achieved, additional material was added until an excess of solid was present.The vials were capped and placed in a shaking incubator which cycled between ambient temperature and 50 0C, changing every 12 hours. Shaking was continued for 4 days. Inspection of the vials showed that the majority of the 1,1,1,3,3,3- hexafluoropropan-2-ol had evaporated, so an additional 500 muL was added. Inspection after another 2 days showed that this vial now contained only a solution, so additional solid (~30mg) was added.A sample of each slurry was transferred to a glass slide, partially dried either by evaporation or by wicker filtration of any excess solvent and examined by XRPD. Recrystallization from l,l,l,3,3,3-hexafluoro-propan-2-ol afforded crystal form G (see above). Under these conditions, recrystallization from acetone, acetonitrile, THF, DMA, DCM, cyclohexane, heptane, n-butanol, DMF, 1,4-dioxane, ethyl acetate, ethanol, butyl acetate, /-propyl acetate, MEK, methanol, MIBK, propan-1-ol, propan-2-ol, t-BME, toluene, water, or NMP afforded crystal form A.
	In N,N-dimethyl-formamide; at 20 - 50℃; for 144.0h;Purification / work up;	Example 11: Recrystallization From Various Solvents500muL of each of 24 solvents were added to 50 mg +/- 5 mg of form A, to produce a saturated solution. If complete dissolution was achieved, additional material was added until an excess of solid was present.The vials were capped and placed in a shaking incubator which cycled between ambient temperature and 50 0C, changing every 12 hours. Shaking was continued for 4 days. Inspection of the vials showed that the majority of the 1,1,1,3,3,3- hexafluoropropan-2-ol had evaporated, so an additional 500 muL was added. Inspection after another 2 days showed that this vial now contained only a solution, so additional solid (~30mg) was added.A sample of each slurry was transferred to a glass slide, partially dried either by evaporation or by wicker filtration of any excess solvent and examined by XRPD. Recrystallization from l,l,l,3,3,3-hexafluoro-propan-2-ol afforded crystal form G (see above). Under these conditions, recrystallization from acetone, acetonitrile, THF, DMA, DCM, cyclohexane, heptane, n-butanol, DMF, 1,4-dioxane, ethyl acetate, ethanol, butyl acetate, /-propyl acetate, MEK, methanol, MIBK, propan-1-ol, propan-2-ol, t-BME, toluene, water, or NMP afforded crystal form A.
	In n-heptane; at 20 - 50℃; for 144.0h;Purification / work up;	Example 11: Recrystallization From Various Solvents500muL of each of 24 solvents were added to 50 mg +/- 5 mg of form A, to produce a saturated solution. If complete dissolution was achieved, additional material was added until an excess of solid was present.The vials were capped and placed in a shaking incubator which cycled between ambient temperature and 50 0C, changing every 12 hours. Shaking was continued for 4 days. Inspection of the vials showed that the majority of the 1,1,1,3,3,3- hexafluoropropan-2-ol had evaporated, so an additional 500 muL was added. Inspection after another 2 days showed that this vial now contained only a solution, so additional solid (~30mg) was added.A sample of each slurry was transferred to a glass slide, partially dried either by evaporation or by wicker filtration of any excess solvent and examined by XRPD. Recrystallization from l,l,l,3,3,3-hexafluoro-propan-2-ol afforded crystal form G (see above). Under these conditions, recrystallization from acetone, acetonitrile, THF, DMA, DCM, cyclohexane, heptane, n-butanol, DMF, 1,4-dioxane, ethyl acetate, ethanol, butyl acetate, /-propyl acetate, MEK, methanol, MIBK, propan-1-ol, propan-2-ol, t-BME, toluene, water, or NMP afforded crystal form A.
	In toluene; at 20 - 50℃; for 144.0h;Purification / work up;	Example 11: Recrystallization From Various Solvents500muL of each of 24 solvents were added to 50 mg +/- 5 mg of form A, to produce a saturated solution. If complete dissolution was achieved, additional material was added until an excess of solid was present.The vials were capped and placed in a shaking incubator which cycled between ambient temperature and 50 0C, changing every 12 hours. Shaking was continued for 4 days. Inspection of the vials showed that the majority of the 1,1,1,3,3,3- hexafluoropropan-2-ol had evaporated, so an additional 500 muL was added. Inspection after another 2 days showed that this vial now contained only a solution, so additional solid (~30mg) was added.A sample of each slurry was transferred to a glass slide, partially dried either by evaporation or by wicker filtration of any excess solvent and examined by XRPD. Recrystallization from l,l,l,3,3,3-hexafluoro-propan-2-ol afforded crystal form G (see above). Under these conditions, recrystallization from acetone, acetonitrile, THF, DMA, DCM, cyclohexane, heptane, n-butanol, DMF, 1,4-dioxane, ethyl acetate, ethanol, butyl acetate, /-propyl acetate, MEK, methanol, MIBK, propan-1-ol, propan-2-ol, t-BME, toluene, water, or NMP afforded crystal form A.
	In cyclohexane; at 20 - 50℃; for 144.0h;Purification / work up;	Example 11: Recrystallization From Various Solvents500muL of each of 24 solvents were added to 50 mg +/- 5 mg of form A, to produce a saturated solution. If complete dissolution was achieved, additional material was added until an excess of solid was present.The vials were capped and placed in a shaking incubator which cycled between ambient temperature and 50 0C, changing every 12 hours. Shaking was continued for 4 days. Inspection of the vials showed that the majority of the 1,1,1,3,3,3- hexafluoropropan-2-ol had evaporated, so an additional 500 muL was added. Inspection after another 2 days showed that this vial now contained only a solution, so additional solid (~30mg) was added.A sample of each slurry was transferred to a glass slide, partially dried either by evaporation or by wicker filtration of any excess solvent and examined by XRPD. Recrystallization from l,l,l,3,3,3-hexafluoro-propan-2-ol afforded crystal form G (see above). Under these conditions, recrystallization from acetone, acetonitrile, THF, DMA, DCM, cyclohexane, heptane, n-butanol, DMF, 1,4-dioxane, ethyl acetate, ethanol, butyl acetate, /-propyl acetate, MEK, methanol, MIBK, propan-1-ol, propan-2-ol, t-BME, toluene, water, or NMP afforded crystal form A.
	In 1,4-dioxane; at 20 - 50℃; for 144.0h;Purification / work up;	Example 11: Recrystallization From Various Solvents500muL of each of 24 solvents were added to 50 mg +/- 5 mg of form A, to produce a saturated solution. If complete dissolution was achieved, additional material was added until an excess of solid was present.The vials were capped and placed in a shaking incubator which cycled between ambient temperature and 50 0C, changing every 12 hours. Shaking was continued for 4 days. Inspection of the vials showed that the majority of the 1,1,1,3,3,3- hexafluoropropan-2-ol had evaporated, so an additional 500 muL was added. Inspection after another 2 days showed that this vial now contained only a solution, so additional solid (~30mg) was added.A sample of each slurry was transferred to a glass slide, partially dried either by evaporation or by wicker filtration of any excess solvent and examined by XRPD. Recrystallization from l,l,l,3,3,3-hexafluoro-propan-2-ol afforded crystal form G (see above). Under these conditions, recrystallization from acetone, acetonitrile, THF, DMA, DCM, cyclohexane, heptane, n-butanol, DMF, 1,4-dioxane, ethyl acetate, ethanol, butyl acetate, /-propyl acetate, MEK, methanol, MIBK, propan-1-ol, propan-2-ol, t-BME, toluene, water, or NMP afforded crystal form A.
	In 1-methyl-pyrrolidin-2-one; at 20 - 50℃; for 144.0h;Purification / work up;	Example 11: Recrystallization From Various Solvents500muL of each of 24 solvents were added to 50 mg +/- 5 mg of form A, to produce a saturated solution. If complete dissolution was achieved, additional material was added until an excess of solid was present.The vials were capped and placed in a shaking incubator which cycled between ambient temperature and 50 0C, changing every 12 hours. Shaking was continued for 4 days. Inspection of the vials showed that the majority of the 1,1,1,3,3,3- hexafluoropropan-2-ol had evaporated, so an additional 500 muL was added. Inspection after another 2 days showed that this vial now contained only a solution, so additional solid (~30mg) was added.A sample of each slurry was transferred to a glass slide, partially dried either by evaporation or by wicker filtration of any excess solvent and examined by XRPD. Recrystallization from l,l,l,3,3,3-hexafluoro-propan-2-ol afforded crystal form G (see above). Under these conditions, recrystallization from acetone, acetonitrile, THF, DMA, DCM, cyclohexane, heptane, n-butanol, DMF, 1,4-dioxane, ethyl acetate, ethanol, butyl acetate, /-propyl acetate, MEK, methanol, MIBK, propan-1-ol, propan-2-ol, t-BME, toluene, water, or NMP afforded crystal form A.
	In butanone; at 20 - 50℃; for 144.0h;Purification / work up;	Example 11: Recrystallization From Various Solvents500muL of each of 24 solvents were added to 50 mg +/- 5 mg of form A, to produce a saturated solution. If complete dissolution was achieved, additional material was added until an excess of solid was present.The vials were capped and placed in a shaking incubator which cycled between ambient temperature and 50 0C, changing every 12 hours. Shaking was continued for 4 days. Inspection of the vials showed that the majority of the 1,1,1,3,3,3- hexafluoropropan-2-ol had evaporated, so an additional 500 muL was added. Inspection after another 2 days showed that this vial now contained only a solution, so additional solid (~30mg) was added.A sample of each slurry was transferred to a glass slide, partially dried either by evaporation or by wicker filtration of any excess solvent and examined by XRPD. Recrystallization from l,l,l,3,3,3-hexafluoro-propan-2-ol afforded crystal form G (see above). Under these conditions, recrystallization from acetone, acetonitrile, THF, DMA, DCM, cyclohexane, heptane, n-butanol, DMF, 1,4-dioxane, ethyl acetate, ethanol, butyl acetate, /-propyl acetate, MEK, methanol, MIBK, propan-1-ol, propan-2-ol, t-BME, toluene, water, or NMP afforded crystal form A.
	In acetonitrile; at 20 - 50℃; for 144.0h;Purification / work up;	Example 11: Recrystallization From Various Solvents500muL of each of 24 solvents were added to 50 mg +/- 5 mg of form A, to produce a saturated solution. If complete dissolution was achieved, additional material was added until an excess of solid was present.The vials were capped and placed in a shaking incubator which cycled between ambient temperature and 50 0C, changing every 12 hours. Shaking was continued for 4 days. Inspection of the vials showed that the majority of the 1,1,1,3,3,3- hexafluoropropan-2-ol had evaporated, so an additional 500 muL was added. Inspection after another 2 days showed that this vial now contained only a solution, so additional solid (~30mg) was added.A sample of each slurry was transferred to a glass slide, partially dried either by evaporation or by wicker filtration of any excess solvent and examined by XRPD. Recrystallization from l,l,l,3,3,3-hexafluoro-propan-2-ol afforded crystal form G (see above). Under these conditions, recrystallization from acetone, acetonitrile, THF, DMA, DCM, cyclohexane, heptane, n-butanol, DMF, 1,4-dioxane, ethyl acetate, ethanol, butyl acetate, /-propyl acetate, MEK, methanol, MIBK, propan-1-ol, propan-2-ol, t-BME, toluene, water, or NMP afforded crystal form A.
	In ethanol; at 20 - 50℃; for 144.0h;Purification / work up;	Example 11: Recrystallization From Various Solvents500muL of each of 24 solvents were added to 50 mg +/- 5 mg of form A, to produce a saturated solution. If complete dissolution was achieved, additional material was added until an excess of solid was present.The vials were capped and placed in a shaking incubator which cycled between ambient temperature and 50 0C, changing every 12 hours. Shaking was continued for 4 days. Inspection of the vials showed that the majority of the 1,1,1,3,3,3- hexafluoropropan-2-ol had evaporated, so an additional 500 muL was added. Inspection after another 2 days showed that this vial now contained only a solution, so additional solid (~30mg) was added.A sample of each slurry was transferred to a glass slide, partially dried either by evaporation or by wicker filtration of any excess solvent and examined by XRPD. Recrystallization from l,l,l,3,3,3-hexafluoro-propan-2-ol afforded crystal form G (see above). Under these conditions, recrystallization from acetone, acetonitrile, THF, DMA, DCM, cyclohexane, heptane, n-butanol, DMF, 1,4-dioxane, ethyl acetate, ethanol, butyl acetate, /-propyl acetate, MEK, methanol, MIBK, propan-1-ol, propan-2-ol, t-BME, toluene, water, or NMP afforded crystal form A.
	In water; at 20 - 50℃; for 144.0h;Purification / work up;	Example 11: Recrystallization From Various Solvents500muL of each of 24 solvents were added to 50 mg +/- 5 mg of form A, to produce a saturated solution. If complete dissolution was achieved, additional material was added until an excess of solid was present.The vials were capped and placed in a shaking incubator which cycled between ambient temperature and 50 0C, changing every 12 hours. Shaking was continued for 4 days. Inspection of the vials showed that the majority of the 1,1,1,3,3,3- hexafluoropropan-2-ol had evaporated, so an additional 500 muL was added. Inspection after another 2 days showed that this vial now contained only a solution, so additional solid (~30mg) was added.A sample of each slurry was transferred to a glass slide, partially dried either by evaporation or by wicker filtration of any excess solvent and examined by XRPD. Recrystallization from l,l,l,3,3,3-hexafluoro-propan-2-ol afforded crystal form G (see above). Under these conditions, recrystallization from acetone, acetonitrile, THF, DMA, DCM, cyclohexane, heptane, n-butanol, DMF, 1,4-dioxane, ethyl acetate, ethanol, butyl acetate, /-propyl acetate, MEK, methanol, MIBK, propan-1-ol, propan-2-ol, t-BME, toluene, water, or NMP afforded crystal form A.
	In Isopropyl acetate; at 20 - 50℃; for 144.0h;Purification / work up;	Example 11: Recrystallization From Various Solvents500muL of each of 24 solvents were added to 50 mg +/- 5 mg of form A, to produce a saturated solution. If complete dissolution was achieved, additional material was added until an excess of solid was present.The vials were capped and placed in a shaking incubator which cycled between ambient temperature and 50 0C, changing every 12 hours. Shaking was continued for 4 days. Inspection of the vials showed that the majority of the 1,1,1,3,3,3- hexafluoropropan-2-ol had evaporated, so an additional 500 muL was added. Inspection after another 2 days showed that this vial now contained only a solution, so additional solid (~30mg) was added.A sample of each slurry was transferred to a glass slide, partially dried either by evaporation or by wicker filtration of any excess solvent and examined by XRPD. Recrystallization from l,l,l,3,3,3-hexafluoro-propan-2-ol afforded crystal form G (see above). Under these conditions, recrystallization from acetone, acetonitrile, THF, DMA, DCM, cyclohexane, heptane, n-butanol, DMF, 1,4-dioxane, ethyl acetate, ethanol, butyl acetate, /-propyl acetate, MEK, methanol, MIBK, propan-1-ol, propan-2-ol, t-BME, toluene, water, or NMP afforded crystal form A.
	In tetrahydrofuran; at 20 - 50℃; for 144.0h;Purification / work up;	Example 11: Recrystallization From Various Solvents500muL of each of 24 solvents were added to 50 mg +/- 5 mg of form A, to produce a saturated solution. If complete dissolution was achieved, additional material was added until an excess of solid was present.The vials were capped and placed in a shaking incubator which cycled between ambient temperature and 50 0C, changing every 12 hours. Shaking was continued for 4 days. Inspection of the vials showed that the majority of the 1,1,1,3,3,3- hexafluoropropan-2-ol had evaporated, so an additional 500 muL was added. Inspection after another 2 days showed that this vial now contained only a solution, so additional solid (~30mg) was added.A sample of each slurry was transferred to a glass slide, partially dried either by evaporation or by wicker filtration of any excess solvent and examined by XRPD. Recrystallization from l,l,l,3,3,3-hexafluoro-propan-2-ol afforded crystal form G (see above). Under these conditions, recrystallization from acetone, acetonitrile, THF, DMA, DCM, cyclohexane, heptane, n-butanol, DMF, 1,4-dioxane, ethyl acetate, ethanol, butyl acetate, /-propyl acetate, MEK, methanol, MIBK, propan-1-ol, propan-2-ol, t-BME, toluene, water, or NMP afforded crystal form A.
	In N,N-dimethyl acetamide; at 20 - 50℃; for 144.0h;Purification / work up;	Example 11: Recrystallization From Various Solvents500muL of each of 24 solvents were added to 50 mg +/- 5 mg of form A, to produce a saturated solution. If complete dissolution was achieved, additional material was added until an excess of solid was present.The vials were capped and placed in a shaking incubator which cycled between ambient temperature and 50 0C, changing every 12 hours. Shaking was continued for 4 days. Inspection of the vials showed that the majority of the 1,1,1,3,3,3- hexafluoropropan-2-ol had evaporated, so an additional 500 muL was added. Inspection after another 2 days showed that this vial now contained only a solution, so additional solid (~30mg) was added.A sample of each slurry was transferred to a glass slide, partially dried either by evaporation or by wicker filtration of any excess solvent and examined by XRPD. Recrystallization from l,l,l,3,3,3-hexafluoro-propan-2-ol afforded crystal form G (see above). Under these conditions, recrystallization from acetone, acetonitrile, THF, DMA, DCM, cyclohexane, heptane, n-butanol, DMF, 1,4-dioxane, ethyl acetate, ethanol, butyl acetate, /-propyl acetate, MEK, methanol, MIBK, propan-1-ol, propan-2-ol, t-BME, toluene, water, or NMP afforded crystal form A.
	In acetic acid butyl ester; at 20 - 50℃; for 144.0h;Purification / work up;	Example 11: Recrystallization From Various Solvents500muL of each of 24 solvents were added to 50 mg +/- 5 mg of form A, to produce a saturated solution. If complete dissolution was achieved, additional material was added until an excess of solid was present.The vials were capped and placed in a shaking incubator which cycled between ambient temperature and 50 0C, changing every 12 hours. Shaking was continued for 4 days. Inspection of the vials showed that the majority of the 1,1,1,3,3,3- hexafluoropropan-2-ol had evaporated, so an additional 500 muL was added. Inspection after another 2 days showed that this vial now contained only a solution, so additional solid (~30mg) was added.A sample of each slurry was transferred to a glass slide, partially dried either by evaporation or by wicker filtration of any excess solvent and examined by XRPD. Recrystallization from l,l,l,3,3,3-hexafluoro-propan-2-ol afforded crystal form G (see above). Under these conditions, recrystallization from acetone, acetonitrile, THF, DMA, DCM, cyclohexane, heptane, n-butanol, DMF, 1,4-dioxane, ethyl acetate, ethanol, butyl acetate, /-propyl acetate, MEK, methanol, MIBK, propan-1-ol, propan-2-ol, t-BME, toluene, water, or NMP afforded crystal form A.
	In propan-1-ol; at 20 - 50℃; for 144.0h;Purification / work up;	Example 11: Recrystallization From Various Solvents500muL of each of 24 solvents were added to 50 mg +/- 5 mg of form A, to produce a saturated solution. If complete dissolution was achieved, additional material was added until an excess of solid was present.The vials were capped and placed in a shaking incubator which cycled between ambient temperature and 50 0C, changing every 12 hours. Shaking was continued for 4 days. Inspection of the vials showed that the majority of the 1,1,1,3,3,3- hexafluoropropan-2-ol had evaporated, so an additional 500 muL was added. Inspection after another 2 days showed that this vial now contained only a solution, so additional solid (~30mg) was added.A sample of each slurry was transferred to a glass slide, partially dried either by evaporation or by wicker filtration of any excess solvent and examined by XRPD. Recrystallization from l,l,l,3,3,3-hexafluoro-propan-2-ol afforded crystal form G (see above). Under these conditions, recrystallization from acetone, acetonitrile, THF, DMA, DCM, cyclohexane, heptane, n-butanol, DMF, 1,4-dioxane, ethyl acetate, ethanol, butyl acetate, /-propyl acetate, MEK, methanol, MIBK, propan-1-ol, propan-2-ol, t-BME, toluene, water, or NMP afforded crystal form A.
	In 4-methyl-2-pentanone; at 20 - 50℃; for 144.0h;Purification / work up;	Example 11: Recrystallization From Various Solvents500muL of each of 24 solvents were added to 50 mg +/- 5 mg of form A, to produce a saturated solution. If complete dissolution was achieved, additional material was added until an excess of solid was present.The vials were capped and placed in a shaking incubator which cycled between ambient temperature and 50 0C, changing every 12 hours. Shaking was continued for 4 days. Inspection of the vials showed that the majority of the 1,1,1,3,3,3- hexafluoropropan-2-ol had evaporated, so an additional 500 muL was added. Inspection after another 2 days showed that this vial now contained only a solution, so additional solid (~30mg) was added.A sample of each slurry was transferred to a glass slide, partially dried either by evaporation or by wicker filtration of any excess solvent and examined by XRPD. Recrystallization from l,l,l,3,3,3-hexafluoro-propan-2-ol afforded crystal form G (see above). Under these conditions, recrystallization from acetone, acetonitrile, THF, DMA, DCM, cyclohexane, heptane, n-butanol, DMF, 1,4-dioxane, ethyl acetate, ethanol, butyl acetate, /-propyl acetate, MEK, methanol, MIBK, propan-1-ol, propan-2-ol, t-BME, toluene, water, or NMP afforded crystal form A.
	In acetone; at 20 - 50℃; for 144.0h;Purification / work up;	Example 11: Recrystallization From Various Solvents500muL of each of 24 solvents were added to 50 mg +/- 5 mg of form A, to produce a saturated solution. If complete dissolution was achieved, additional material was added until an excess of solid was present.The vials were capped and placed in a shaking incubator which cycled between ambient temperature and 50 0C, changing every 12 hours. Shaking was continued for 4 days. Inspection of the vials showed that the majority of the 1,1,1,3,3,3- hexafluoropropan-2-ol had evaporated, so an additional 500 muL was added. Inspection after another 2 days showed that this vial now contained only a solution, so additional solid (~30mg) was added.A sample of each slurry was transferred to a glass slide, partially dried either by evaporation or by wicker filtration of any excess solvent and examined by XRPD. Recrystallization from l,l,l,3,3,3-hexafluoro-propan-2-ol afforded crystal form G (see above). Under these conditions, recrystallization from acetone, acetonitrile, THF, DMA, DCM, cyclohexane, heptane, n-butanol, DMF, 1,4-dioxane, ethyl acetate, ethanol, butyl acetate, /-propyl acetate, MEK, methanol, MIBK, propan-1-ol, propan-2-ol, t-BME, toluene, water, or NMP afforded crystal form A.
	In methanol; at 20 - 50℃; for 144.0h;Purification / work up;	Example 11: Recrystallization From Various Solvents500muL of each of 24 solvents were added to 50 mg +/- 5 mg of form A, to produce a saturated solution. If complete dissolution was achieved, additional material was added until an excess of solid was present.The vials were capped and placed in a shaking incubator which cycled between ambient temperature and 50 0C, changing every 12 hours. Shaking was continued for 4 days. Inspection of the vials showed that the majority of the 1,1,1,3,3,3- hexafluoropropan-2-ol had evaporated, so an additional 500 muL was added. Inspection after another 2 days showed that this vial now contained only a solution, so additional solid (~30mg) was added.A sample of each slurry was transferred to a glass slide, partially dried either by evaporation or by wicker filtration of any excess solvent and examined by XRPD. Recrystallization from l,l,l,3,3,3-hexafluoro-propan-2-ol afforded crystal form G (see above). Under these conditions, recrystallization from acetone, acetonitrile, THF, DMA, DCM, cyclohexane, heptane, n-butanol, DMF, 1,4-dioxane, ethyl acetate, ethanol, butyl acetate, /-propyl acetate, MEK, methanol, MIBK, propan-1-ol, propan-2-ol, t-BME, toluene, water, or NMP afforded crystal form A.
	In t-BME; at 20 - 50℃; for 144.0h;Purification / work up;	Example 11: Recrystallization From Various Solvents500muL of each of 24 solvents were added to 50 mg +/- 5 mg of form A, to produce a saturated solution. If complete dissolution was achieved, additional material was added until an excess of solid was present.The vials were capped and placed in a shaking incubator which cycled between ambient temperature and 50 0C, changing every 12 hours. Shaking was continued for 4 days. Inspection of the vials showed that the majority of the 1,1,1,3,3,3- hexafluoropropan-2-ol had evaporated, so an additional 500 muL was added. Inspection after another 2 days showed that this vial now contained only a solution, so additional solid (~30mg) was added.A sample of each slurry was transferred to a glass slide, partially dried either by evaporation or by wicker filtration of any excess solvent and examined by XRPD. Recrystallization from l,l,l,3,3,3-hexafluoro-propan-2-ol afforded crystal form G (see above). Under these conditions, recrystallization from acetone, acetonitrile, THF, DMA, DCM, cyclohexane, heptane, n-butanol, DMF, 1,4-dioxane, ethyl acetate, ethanol, butyl acetate, /-propyl acetate, MEK, methanol, MIBK, propan-1-ol, propan-2-ol, t-BME, toluene, water, or NMP afforded crystal form A.

2
[ 123-91-1 ]
[ 442908-10-3 ]
3-(4-amino-3-methylbenzyl)-7-(furan-2-yl)-3H-[1,2,3]triazolo[4,5-d]pyrimidin-5-amine 1,4-dioxane hemisolvate [ No CAS ]

Yield	Reaction Conditions	Operation in experiment
		Example 8: Characterization of Crystal Form E ofl (1,4-dioxane solvate) A sample of 1 in crystal form E was prepared by recrystallization from 1,4- dioxane. The sample was characterized by XRPD, DSC, and TGA. FIG. 4A shows an XRPD trace of crystal form E. The XRPD pattern of crystal form E is characterized by peaks at 2Theta of 8.49 , 8.84, 9.50, 11.60, 13.73, 14.99, 15.56, 16.95, 17.77, 19.03, 19.96, 22.70, 23.83, 24.05, 25.51, and 26.57. FIG. 4B shows a DSC thermogram for crystal form E. DSC thermograms of crystal form E show a desolvation endotherm above 123 0C, and a minimum in (i.e., melting point) at about 244 0C. The melting point of desolvated form E suggests that form E converts to form A upon desolvation. FIG. 4C shows a TGA trace for crystal form E. TGA revealed that form E lost13% of its weight upon heating from ambient temperature to 50 0C, or 0.6 moles solvent per mole of 1, consistent with form D being a 1,4-dioxane hemisolvate.

Reference： [1]Patent: WO2008/86201,2008,A1 .Location in patent: Page/Page column 24

3
[ 442908-10-3 ]
[ 78-93-3 ]
3-(4-amino-3-methylbenzyl)-7-(furan-2-yl)-3H-[1,2,3]triazolo[4,5-d]pyrimidin-5-amine methyl ethyl ketone solvate [ No CAS ]

Yield	Reaction Conditions	Operation in experiment
		Example 9: Characterization of Crystal Form F ofl (methyl ethyl ketone solvate) A sample of 1 in crystal form F was prepared by recrystallization from methyl ethyl ketone (MEK). The sample was characterized by XRPD and DSC. FIG. 5A shows an XRPD trace of crystal form F. The XRPD pattern of crystal form F is characterized by peaks at 2Theta of 8.44, 8.78, 9.48, 11.60, 13.66, 14.94, 15.43, 17.00, 17.70, 18.94, 19.76, 20.00, 22.35, 23.83, 25.40, 25.62, 26.26, and 26.68. FIG. 5B shows a DSC thermogram for crystal form F. DSC thermograms of crystal form E show a desolvation endotherm above 102 0C, and a minimum in (i.e., melting point) at about 240 0C. The melting point of desolvated form F suggests that form F converts to form A upon desolvation.

Reference： [1]Patent: WO2008/86201,2008,A1 .Location in patent: Page/Page column 24

4
[ 920-66-1 ]
[ 442908-10-3 ]
3-(4-amino-3-methylbenzyl)-7-(furan-2-yl)-3H-[1,2,3]triazolo[4,5-d]pyrimidin-5-amine 1,1,1,3,3,3-hexafluoropropan-2-ol solvate [ No CAS ]

Yield	Reaction Conditions	Operation in experiment
	at 20 - 50℃; for 144.0h;Product distribution / selectivity;	Example 10: Characterization of Crystal Form G ofl (hexafluoroisopropanol solvate)A sample of 1 in crystal form G was prepared by recrystallization from l,l,l,3,3,3-hexafluoropropan-2-ol. The sample was characterized by XRPD, DSC, and <n="26"/>TGA. FIG. 6A shows an XRPD trace of crystal form G. The XRPD pattern of crystal form G is characterized by peaks at 2Theta of 4.66, 6.56, 10.06, 10.81, 12.00, 13.31, 14.74, 16.00, 16.51, 17.40, 18.79, 19.56, 20.31, 21.71, and 22.59. FIG. 6B shows a DSC thermogram for crystal form G. DSC thermograms of crystal form G show a desolvation endotherm above 84 0C, and a minimum in (i.e., melting point) at about 241 0C. The melting point of desolvated form G suggests that form G converts to form A upon desolvation.FIG. 6C shows a TGA trace for crystal form G. TGA revealed that form G lost 40% of its weight upon heating from ambient temperature to 50 0C, or 1.3 moles solvent per mole of 1, consistent with form G being a hexafluoroisopropanol solvate.FIG. 6D shows variable temperature XRPD traces of crystal form G. Traces (from bottom to top) were recorded at ambient temperature, 25 0C, 70 0C, 100 0C, 120 0C, 210 0C, 220 0C, 230 0C, 235C, and 240 0C. Note that the traces recorded above 200 0C showed additional signals due to the presence of a protective semi-transparent dome. The final product was crystal form B. Example 11: Recrystallization From Various Solvents500muL of each of 24 solvents were added to 50 mg +/- 5 mg of form A, to produce a saturated solution. If complete dissolution was achieved, additional material was added until an excess of solid was present.The vials were capped and placed in a shaking incubator which cycled between ambient temperature and 50 0C, changing every 12 hours. Shaking was continued for 4 days. Inspection of the vials showed that the majority of the 1,1,1,3,3,3- hexafluoropropan-2-ol had evaporated, so an additional 500 muL was added. Inspection after another 2 days showed that this vial now contained only a solution, so additional solid (~30mg) was added.A sample of each slurry was transferred to a glass slide, partially dried either by evaporation or by wicker filtration of any excess solvent and examined by XRPD. Recrystallization from l,l,l,3,3,3-hexafluoro-propan-2-ol afforded crystal form G (see above). Under these conditions, recrystallization from acetone, acetonitrile, THF, DMA, DCM, cyclohexane, heptane, n-butanol, DMF, 1,4-dioxane, ethyl acetate, ethanol, butyl acetate, /-propyl acetate, MEK, methanol, MIBK, propan-1-ol, propan-2-ol, t-BME, toluene, water, or NMP afforded crystal form A.

Reference： [1]Patent: WO2008/86201,2008,A1 .Location in patent: Page/Page column 24-25

5
[ 109-99-9 ]
[ 442908-10-3 ]
3-(4-amino-3-methylbenzyl)-7-(furan-2-yl)-3H-[1,2,3]triazolo[4,5-d]pyrimidin-5-amine tetrahydrofurane hemisolvate [ No CAS ]

Yield	Reaction Conditions	Operation in experiment
	Heating / reflux;	Example 7: Characterization of Crystal Form D ofl (THF solvate)A sample of 1 in crystal form D was prepared by recystallization from hot THF. The sample was characterized by XRPD and TGA. FIG. 3A shows the XRPD trace of Form D, which is characterized by peaks at 2Theta of 8.49, 9.00, 9.55, 11.85, 14.04, 15.01, 15.78, 17.13, 18.13, 19.21, 19.50, 20.20, 23.14, 24.23, 24.51, 26.46, and 26.81. FIG. 3B shows a TGA trace for crystal form D. TGA revealed that form D lost 12.5% of its weight upon heating from ambient temperature to 65 0C, or 0.7 moles solvent per mole of 1, consistent with form D being a THF hemisolvate. <n="25"/>FIG. 3 C shows variable temperature XRPD traces of crystal form D. Traces (from bottom to top) were recorded at ambient temperature, 50 0C, 65 0C, 115 0C, 140 0C, 170 0C, after cooling to 140 0C, and after cooling to 30 0C. The final product was crystal form A.
		Example 12: Characterization of Crystal Form H of 1 (THF solvate)A sample of 1 in crystal form H was prepared by recystallization from THF. The sample was characterized by XRPD and TGA. FIG. 7A shows the XRPD trace of Form H, which is characterized by peaks at 2Theta of 8.40, 8.82, 9.33, 13.67, 14.21, 14.74, 15.43, 16.88, 17.88, 19.06, 19.73, 23.96, 25.36, 25.99, and 26.45. FIG. 7B shows a TGA trace for crystal form H. TGA revealed that form H lost 38% of its weight upon heating from ambient temperature to 150 0C, consistent with form H being a THF hemisolvate.

Reference： [1]Patent: WO2008/86201,2008,A1 .Location in patent: Page/Page column 23-24
[2]Patent: WO2008/86201,2008,A1 .Location in patent: Page/Page column 26

6
[ 442908-07-8 ]
[ 442908-10-3 ]

Yield	Reaction Conditions	Operation in experiment
92%	With formic acid; triethylamine;5% palladium over charcoal; In tetrahydrofuran; at 70℃; for 5.0h;	Example 4: Preparation of3-(4-amino-3-methylbenzyl)-7-(furan-2-yl)-3H- [l,2,3]triazolo[4,5-d]pyrimidin-5-amine (1) A 250 mL 2-necked round-bottomed flask was charged with 7-(furan-2-yl)-3-(3- methyl-4-nitrobenzyl)-3H-[l,2,3]triazolo[4,5-d]pyrimidin-5-amine (3.0 g, 8.5 mmol) and 5% Pd/C catalyst (0.46 g, 0.073 mmol) under a nitrogen atmosphere. Next, THF (72 mL) and triethylamine (9.0 mL, 65 mmol) were added via syringe and the resulting mixture was stirred to obtain slurry. Formic acid (2.3 mL, 46.03 mmol) was then added all at once, and the mixture was heated with a bath set to a temperature of 70 0C. After 5 hours the reaction was cooled to 25 0C. Water (60 mL) was added, and concentrated hydrochloric acid was added dropwise to dissolve the product. The solution was filtered through Celite 545 to remove the catalyst, and the filter cake was washed with additional water (2 X 5 mL). To the yellowish filtrate was added 50% sodium hydroxide in water to precipitate the product. The mixture was stirred for an additional hour before isolation by filtration. The filter cake was washed with water (10 mL) then methanol (10 mL). The product was dried under vacuum to constant weight to yield 2.79 g (92%) of 3-(4-amino- 3-methylbenzyl)-7-(furan-2-yl)-3H-[l,2,3]triazolo[4,5-d]pyrimidin-5-amine.

Reference： [1]Patent: WO2008/86201,2008,A1 .Location in patent: Page/Page column 21
[2]Journal of Medicinal Chemistry,2009,vol. 52,p. 33 - 47

Yield	Reaction Conditions	Operation in experiment
	In 1-methyl-pyrrolidin-2-one; at 20℃; for 552.0h;Reactivity (does not react);	Example 13: Relative Stability of Forms A and BThe relative stabilities of the forms A and B was determined by a vapour diffusion experiment. Approximately equal amounts of the two forms were ground together to produce an intimate mixture. The mixture was packed into a silicon 510-cut recessed wafer XRPD holder and the XRPD of the mixture determined. The holder was then placed in a covered dish containing NMP (a known solvent 1) at room temperature. The mixture was re-examined from time to time to monitor any changes in the XRPD pattern.FIG. 8 shows that over time the peaks characteristic of Form B diminish, disappearing complete by the 23 day time point. This indicated that at room temperature, Form A was the more stable polymorph. The traces from bottom to top in FIG. 8 were recorded initially, at 24 hours, at 3 days, at 1 week, at 10 days, and at 23 days; the topmost traces are a form A reference and a form B reference.

8
3-(4-amino-3-methylbenzyl)-7-(furan-2-yl)-3H-[1,2,3]triazolo[4,5-d]pyrimidin-5-amine tetrahydrofurane hemisolvate [ No CAS ]
[ 442908-10-3 ]

Yield	Reaction Conditions	Operation in experiment
	at 20 - 170℃;Product distribution / selectivity;	Example 7: Characterization of Crystal Form D ofl (THF solvate)A sample of 1 in crystal form D was prepared by recystallization from hot THF. The sample was characterized by XRPD and TGA. FIG. 3A shows the XRPD trace of Form D, which is characterized by peaks at 2Theta of 8.49, 9.00, 9.55, 11.85, 14.04, 15.01, 15.78, 17.13, 18.13, 19.21, 19.50, 20.20, 23.14, 24.23, 24.51, 26.46, and 26.81. FIG. 3B shows a TGA trace for crystal form D. TGA revealed that form D lost 12.5% of its weight upon heating from ambient temperature to 65 0C, or 0.7 moles solvent per mole of 1, consistent with form D being a THF hemisolvate. <n="25"/>FIG. 3 C shows variable temperature XRPD traces of crystal form D. Traces (from bottom to top) were recorded at ambient temperature, 50 0C, 65 0C, 115 0C, 140 0C, 170 0C, after cooling to 140 0C, and after cooling to 30 0C. The final product was crystal form A.

Reference： [1]Patent: WO2008/86201,2008,A1 .Location in patent: Page/Page column 23-24

9
3-(4-amino-3-methylbenzyl)-7-(furan-2-yl)-3H-[1,2,3]triazolo[4,5-d]pyrimidin-5-amine 1,1,1,3,3,3-hexafluoropropan-2-ol solvate [ No CAS ]
[ 442908-10-3 ]

Yield	Reaction Conditions	Operation in experiment
	at 20 - 240℃;Product distribution / selectivity;	Example 10: Characterization of Crystal Form G ofl (hexafluoroisopropanol solvate)A sample of 1 in crystal form G was prepared by recrystallization from l,l,l,3,3,3-hexafluoropropan-2-ol. The sample was characterized by XRPD, DSC, and <n="26"/>TGA. FIG. 6A shows an XRPD trace of crystal form G. The XRPD pattern of crystal form G is characterized by peaks at 2Theta of 4.66, 6.56, 10.06, 10.81, 12.00, 13.31, 14.74, 16.00, 16.51, 17.40, 18.79, 19.56, 20.31, 21.71, and 22.59. FIG. 6B shows a DSC thermogram for crystal form G. DSC thermograms of crystal form G show a desolvation endotherm above 84 0C, and a minimum in (i.e., melting point) at about 241 0C. The melting point of desolvated form G suggests that form G converts to form A upon desolvation.FIG. 6C shows a TGA trace for crystal form G. TGA revealed that form G lost 40% of its weight upon heating from ambient temperature to 50 0C, or 1.3 moles solvent per mole of 1, consistent with form G being a hexafluoroisopropanol solvate.FIG. 6D shows variable temperature XRPD traces of crystal form G. Traces (from bottom to top) were recorded at ambient temperature, 25 0C, 70 0C, 100 0C, 120 0C, 210 0C, 220 0C, 230 0C, 235C, and 240 0C. Note that the traces recorded above 200 0C showed additional signals due to the presence of a protective semi-transparent dome. The final product was crystal form B.

Reference： [1]Patent: WO2008/86201,2008,A1 .Location in patent: Page/Page column 24-25

10
[ 442906-78-7 ]
[ 141281-38-1 ]
[ 442908-10-3 ]

Reference： [1]Journal of Medicinal Chemistry,2009,vol. 52,p. 33 - 47

Same Skeleton Products

Related Products

Historical Records

Purity	Size	Price	VIP Price	USA Stock *0-1 Day	Global Stock *5-7 Days	Quantity
{[ item.p_purity ]}	{[ item.pr_size ]}	{[ getRatePrice(item.pr_usd, 1,1) ]} {[ getRatePrice(item.pr_usd,item.pr_rate,item.mem_rate) ]}	{[ getRatePrice(item.pr_usd, 1,1) ]}	Inquiry {[ getRatePrice(item.pr_usd,item.pr_rate,item.mem_rate) ]} {[ getRatePrice(item.pr_usd,1,item.mem_rate) ]}	{[ item.pr_usastock ]}	Inquiry -	{[ item.pr_chinastock ]}	Inquiry -

Precautionary Statements-General
Code	Phrase
P101	If medical advice is needed,have product container or label at hand.
P102	Keep out of reach of children.
P103	Read label before use
Prevention
Code	Phrase
P201	Obtain special instructions before use.
P202	Do not handle until all safety precautions have been read and understood.
P210	Keep away from heat/sparks/open flames/hot surfaces. - No smoking.
P211	Do not spray on an open flame or other ignition source.
P220	Keep/Store away from clothing/combustible materials.
P221	Take any precaution to avoid mixing with combustibles
P222	Do not allow contact with air.
P223	Keep away from any possible contact with water, because of violent reaction and possible flash fire.
P230	Keep wetted
P231	Handle under inert gas.
P232	Protect from moisture.
P233	Keep container tightly closed.
P234	Keep only in original container.
P235	Keep cool
P240	Ground/bond container and receiving equipment.
P241	Use explosion-proof electrical/ventilating/lighting/equipment.
P242	Use only non-sparking tools.
P243	Take precautionary measures against static discharge.
P244	Keep reduction valves free from grease and oil.
P250	Do not subject to grinding/shock/friction.
P251	Pressurized container: Do not pierce or burn, even after use.
P260	Do not breathe dust/fume/gas/mist/vapours/spray.
P261	Avoid breathing dust/fume/gas/mist/vapours/spray.
P262	Do not get in eyes, on skin, or on clothing.
P263	Avoid contact during pregnancy/while nursing.
P264	Wash hands thoroughly after handling.
P265	Wash skin thouroughly after handling.
P270	Do not eat, drink or smoke when using this product.
P271	Use only outdoors or in a well-ventilated area.
P272	Contaminated work clothing should not be allowed out of the workplace.
P273	Avoid release to the environment.
P280	Wear protective gloves/protective clothing/eye protection/face protection.
P281	Use personal protective equipment as required.
P282	Wear cold insulating gloves/face shield/eye protection.
P283	Wear fire/flame resistant/retardant clothing.
P284	Wear respiratory protection.
P285	In case of inadequate ventilation wear respiratory protection.
P231 + P232	Handle under inert gas. Protect from moisture.
P235 + P410	Keep cool. Protect from sunlight.
Response
Code	Phrase
P301	IF SWALLOWED:
P304	IF INHALED:
P305	IF IN EYES:
P306	IF ON CLOTHING:
P307	IF exposed:
P308	IF exposed or concerned:
P309	IF exposed or if you feel unwell:
P310	Immediately call a POISON CENTER or doctor/physician.
P311	Call a POISON CENTER or doctor/physician.
P312	Call a POISON CENTER or doctor/physician if you feel unwell.
P313	Get medical advice/attention.
P314	Get medical advice/attention if you feel unwell.
P315	Get immediate medical advice/attention.
P320
P302 + P352	IF ON SKIN: wash with plenty of soap and water.
P321
P322
P330	Rinse mouth.
P331	Do NOT induce vomiting.
P332	IF SKIN irritation occurs:
P333	If skin irritation or rash occurs:
P334	Immerse in cool water/wrap n wet bandages.
P335	Brush off loose particles from skin.
P336	Thaw frosted parts with lukewarm water. Do not rub affected area.
P337	If eye irritation persists:
P338	Remove contact lenses, if present and easy to do. Continue rinsing.
P340	Remove victim to fresh air and keep at rest in a position comfortable for breathing.
P341	If breathing is difficult, remove victim to fresh air and keep at rest in a position comfortable for breathing.
P342	If experiencing respiratory symptoms:
P350	Gently wash with plenty of soap and water.
P351	Rinse cautiously with water for several minutes.
P352	Wash with plenty of soap and water.
P353	Rinse skin with water/shower.
P360	Rinse immediately contaminated clothing and skin with plenty of water before removing clothes.
P361	Remove/Take off immediately all contaminated clothing.
P362	Take off contaminated clothing and wash before reuse.
P363	Wash contaminated clothing before reuse.
P370	In case of fire:
P371	In case of major fire and large quantities:
P372	Explosion risk in case of fire.
P373	DO NOT fight fire when fire reaches explosives.
P374	Fight fire with normal precautions from a reasonable distance.
P376	Stop leak if safe to do so. Oxidising gases (section 2.4) 1
P377	Leaking gas fire: Do not extinguish, unless leak can be stopped safely.
P378
P380	Evacuate area.
P381	Eliminate all ignition sources if safe to do so.
P390	Absorb spillage to prevent material damage.
P391	Collect spillage. Hazardous to the aquatic environment
P301 + P310	IF SWALLOWED: Immediately call a POISON CENTER or doctor/physician.
P301 + P312	IF SWALLOWED: call a POISON CENTER or doctor/physician IF you feel unwell.
P301 + P330 + P331	IF SWALLOWED: Rinse mouth. Do NOT induce vomiting.
P302 + P334	IF ON SKIN: Immerse in cool water/wrap in wet bandages.
P302 + P350	IF ON SKIN: Gently wash with plenty of soap and water.
P303 + P361 + P353	IF ON SKIN (or hair): Remove/Take off Immediately all contaminated clothing. Rinse SKIN with water/shower.
P304 + P312	IF INHALED: Call a POISON CENTER or doctor/physician if you feel unwell.
P304 + P340	IF INHALED: Remove victim to fresh air and Keep at rest in a position comfortable for breathing.
P304 + P341	IF INHALED: If breathing is difficult, remove victim to fresh air and keep at rest in a position comfortable for breathing.
P305 + P351 + P338	IF IN EYES: Rinse cautiously with water for several minutes. Remove contact lenses, if present and easy to do. Continue rinsing.
P306 + P360	IF ON CLOTHING: Rinse Immediately contaminated CLOTHING and SKIN with plenty of water before removing clothes.
P307 + P311	IF exposed: call a POISON CENTER or doctor/physician.
P308 + P313	IF exposed or concerned: Get medical advice/attention.
P309 + P311	IF exposed or if you feel unwell: call a POISON CENTER or doctor/physician.
P332 + P313	IF SKIN irritation occurs: Get medical advice/attention.
P333 + P313	IF SKIN irritation or rash occurs: Get medical advice/attention.
P335 + P334	Brush off loose particles from skin. Immerse in cool water/wrap in wet bandages.
P337 + P313	IF eye irritation persists: Get medical advice/attention.
P342 + P311	IF experiencing respiratory symptoms: call a POISON CENTER or doctor/physician.
P370 + P376	In case of fire: Stop leak if safe to Do so.
P370 + P378	In case of fire:
P370 + P380	In case of fire: Evacuate area.
P370 + P380 + P375	In case of fire: Evacuate area. Fight fire remotely due to the risk of explosion.
P371 + P380 + P375	In case of major fire and large quantities: Evacuate area. Fight fire remotely due to the risk of explosion.
Storage
Code	Phrase
P401
P402	Store in a dry place.
P403	Store in a well-ventilated place.
P404	Store in a closed container.
P405	Store locked up.
P406	Store in corrosive resistant/ container with a resistant inner liner.
P407	Maintain air gap between stacks/pallets.
P410	Protect from sunlight.
P411
P412	Do not expose to temperatures exceeding 50 oC/ 122 oF.
P413
P420	Store away from other materials.
P422
P402 + P404	Store in a dry place. Store in a closed container.
P403 + P233	Store in a well-ventilated place. Keep container tightly closed.
P403 + P235	Store in a well-ventilated place. Keep cool.
P410 + P403	Protect from sunlight. Store in a well-ventilated place.
P410 + P412	Protect from sunlight. Do not expose to temperatures exceeding 50 oC/122oF.
P411 + P235	Keep cool.
Disposal
Code	Phrase
P501	Dispose of contents/container to ...
P502	Refer to manufacturer/supplier for information on recovery/recycling

Physical hazards
Code	Phrase
H200	Unstable explosive
H201	Explosive; mass explosion hazard
H202	Explosive; severe projection hazard
H203	Explosive; fire, blast or projection hazard
H204	Fire or projection hazard
H205	May mass explode in fire
H220	Extremely flammable gas
H221	Flammable gas
H222	Extremely flammable aerosol
H223	Flammable aerosol
H224	Extremely flammable liquid and vapour
H225	Highly flammable liquid and vapour
H226	Flammable liquid and vapour
H227	Combustible liquid
H228	Flammable solid
H229	Pressurized container: may burst if heated
H230	May react explosively even in the absence of air
H231	May react explosively even in the absence of air at elevated pressure and/or temperature
H240	Heating may cause an explosion
H241	Heating may cause a fire or explosion
H242	Heating may cause a fire
H250	Catches fire spontaneously if exposed to air
H251	Self-heating; may catch fire
H252	Self-heating in large quantities; may catch fire
H260	In contact with water releases flammable gases which may ignite spontaneously
H261	In contact with water releases flammable gas
H270	May cause or intensify fire; oxidizer
H271	May cause fire or explosion; strong oxidizer
H272	May intensify fire; oxidizer
H280	Contains gas under pressure; may explode if heated
H281	Contains refrigerated gas; may cause cryogenic burns or injury
H290	May be corrosive to metals
Health hazards
Code	Phrase
H300	Fatal if swallowed
H301	Toxic if swallowed
H302	Harmful if swallowed
H303	May be harmful if swallowed
H304	May be fatal if swallowed and enters airways
H305	May be harmful if swallowed and enters airways
H310	Fatal in contact with skin
H311	Toxic in contact with skin
H312	Harmful in contact with skin
H313	May be harmful in contact with skin
H314	Causes severe skin burns and eye damage
H315	Causes skin irritation
H316	Causes mild skin irritation
H317	May cause an allergic skin reaction
H318	Causes serious eye damage
H319	Causes serious eye irritation
H320	Causes eye irritation
H330	Fatal if inhaled
H331	Toxic if inhaled
H332	Harmful if inhaled
H333	May be harmful if inhaled
H334	May cause allergy or asthma symptoms or breathing difficulties if inhaled
H335	May cause respiratory irritation
H336	May cause drowsiness or dizziness
H340	May cause genetic defects
H341	Suspected of causing genetic defects
H350	May cause cancer
H351	Suspected of causing cancer
H360	May damage fertility or the unborn child
H361	Suspected of damaging fertility or the unborn child
H361d	Suspected of damaging the unborn child
H362	May cause harm to breast-fed children
H370	Causes damage to organs
H371	May cause damage to organs
H372	Causes damage to organs through prolonged or repeated exposure
H373	May cause damage to organs through prolonged or repeated exposure
Environmental hazards
Code	Phrase
H400	Very toxic to aquatic life
H401	Toxic to aquatic life
H402	Harmful to aquatic life
H410	Very toxic to aquatic life with long-lasting effects
H411	Toxic to aquatic life with long-lasting effects
H412	Harmful to aquatic life with long-lasting effects
H413	May cause long-lasting harmful effects to aquatic life
H420	Harms public health and the environment by destroying ozone in the upper atmosphere

[ CAS No. 442908-10-3 ] {[proInfo.proName]}

Quality Control of [ 442908-10-3 ]

Related Doc. of [ 442908-10-3 ]

Product Details of [ 442908-10-3 ]

Calculated chemistry of [ 442908-10-3 ]

Physicochemical Properties

Pharmacokinetics

Lipophilicity

Druglikeness

Water Solubility

Medicinal Chemistry

Safety of [ 442908-10-3 ]

Application In Synthesis of [ 442908-10-3 ]

[ 442908-10-3 ] Synthesis Path-Upstream 1~2

[ 442908-10-3 ] Synthesis Path-Downstream 1~10

Precautionary Statements-General

Prevention

Response

Storage

Disposal

Physical hazards

Health hazards

Environmental hazards

Inquiry