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Quality Control of [ 1258298-00-8 ]

COA NMR CNMR HPLC LC-MS

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Product Details of [ 1258298-00-8 ]

CAS No. :	1258298-00-8	MDL No. :	MFCD22690823
Formula :	C₁₂H₇BrCl₂N₂O	Boiling Point :	-
Linear Structure Formula :	-	InChI Key :	-
M.W :	346.01	Pubchem ID :	-
Synonyms :

Safety of [ 1258298-00-8 ]

Signal Word:		Class:
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Application In Synthesis of [ 1258298-00-8 ]

* 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.

Downstream synthetic route of [ 1258298-00-8 ]

[ 1258298-00-8 ] Synthesis Path-Downstream 1~13

1
[ 7598-35-8 ]
[ 4659-45-4 ]
[ 1258298-00-8 ]

Yield	Reaction Conditions	Operation in experiment
74%		A solution of <strong>[7598-35-8]2-bromopyridin-4-amine</strong> (0.74 g, 4.3 mmol) in DMF (5 mL) was added to a cooled (0 C.) mixture of NaH (0.31 g, 7.82 mmol, 60% in mineral oil) in DMF (15 mL). The resulting mixture was stirred for 20 minutes at 0 C. and then a solution of 2,6-dichlorobenzoyl chloride (0.82 g, 3.91 mmol) in DMF (5 mL) was added dropwise. The reaction was stirred at 0 C. for 4 hours and then poured onto ice-water (20 mL). The precipitate was collected and filtrate was extracted by EtOAc (2×50 mL). The combined organic extracts were dried over Na2SO4 and concentrated under reduced pressure. The resulting solid was combined with the precipitate to afford N-(2-bromopyridin-4-yl)-2,6-dichlorobenzamide (1.0 g, Yield: 74%). 1HNMR (DMSO-d6, 400 MHz): delta 11.41 (s, 1H), 8.33 (d, J=5.6 Hz, 1H), 7.99 (d, J=1.6 Hz, 1H), 7.64-7.54 (m, 4H). LCMS (ESI) m/z: 345.0 [M+H+].
		To a round-bottom flask was added sodium hydride (0.31g, 7.82mmol, 60% in mineral oil) and N,N-dimethylformamide (15mL). The resulting suspension was cooled to 0C under nitrogen and then <strong>[7598-35-8]2-bromopyridin-4-amine</strong> (0.74g, 4.3mmol) was added. The mixture was stirred at 0C for 20min and then 2,6-dichlorobenzoyl chloride (0.82g, 3.91mmol) was added dropwise. The reaction was warmed to room temperature, stirred for 12h, and then poured into ice-water (20mL). The mixture was extracted with ethyl acetate (2×50mL). The combined organic extracts were dried over Na2SO4 and concentrated under reduced pressure to afford crude desired product (1.0g, 74% yield) that could be used without further purification. 1H NMR (DMSO-d6, 400MHz): delta 11.41 (s, 1H), 8.33 (d, J=5.6Hz, 1H), 7.99 (d, J=1.6Hz, 1H), 7.64-7.54 (m, 4H). LCMS (ESI) m/z=345.0 [M+H]+.

Reference： [1]Patent: US2010/317643,2010,A1 .Location in patent: Page/Page column 49
[2]Journal of Medicinal Chemistry,2014,vol. 57,p. 10176 - 10191
[3]Journal of Medicinal Chemistry,2013,vol. 56,p. 4521 - 4536
[4]European Journal of Medicinal Chemistry,2013,vol. 67,p. 175 - 187

2
[ 108-52-1 ]
[ 1258298-00-8 ]
[ 1258294-01-7 ]

Yield	Reaction Conditions	Operation in experiment
12%	With caesium carbonate In 1,4-dioxane at 140℃; for 3h; Microwave irradiation; Inert atmosphere;	227 To a microwave tube were added N-(2-bromopyridin-4-yl)-2,6-dichlorobenzamide (0.15 g, 0.43 mmol), 2-amino-4-methylpyrimidine (0.056 g, 0.52 mmol), Pd2(dba)3 (0.040 g, 0.043 mmol), XantPhos (0.050 g, 0.087 mmol), Cs2CO3 (0.28 g, 0.87 mmol) and dioxane (2 mL). The mixture was degassed with N2 for 10 min. The resulting mixture was irradiated in a microwave reactor at 140° C. for 3 hours and then cooled to room temperature. The mixture was filtered through Celite and concentrated under reduced pressure. The residue was dissolved in DMF and purified by prep-HPLC (Gilson GX 281, Shim-pack PRC-ODS 250 mm×20 mm×2, gradient: CH3CN/10 mm/L NH4HCO3, 17 min) to give the desired product as a white solid (19 mg, yield: 12%). 1H NMR (500 MHz, MeOH-d4): δ 8.88 (s, 1H), 8.36 (d, J=5.5 Hz, 1H), 8.16 (d, J=6.0 Hz, 1H), 7.64 (s, 1H), 7.45-7.38 (m, 4H), 6.85 (d, J=5.5 Hz, 1H), 2.50 (s, 3H). LCMS (ESI) m/z: 374.0 [M+H+].

Reference： [1]Current Patent Assignee: ROCHE HOLDING AG - US2010/317643, 2010, A1 Location in patent: Page/Page column 97

3
[ 4570-45-0 ]
[ 1258298-00-8 ]
[ 1258294-03-9 ]

Yield	Reaction Conditions	Operation in experiment
9%	With caesium carbonate;tris-(dibenzylideneacetone)dipalladium(0); 4,5-bis(diphenylphos4,5-bis(diphenylphosphino)-9,9-dimethylxanthenephino)-9,9-dimethylxanthene; In 1,4-dioxane; at 140℃; for 3h;Microwave irradiation; Inert atmosphere;	To a microwave tube was added N-(2-bromopyridin-4-yl)-2,6-dichlorobenzamide (0.30 g, 0.87 mmol), 2-aminooxazole (0.11 g, 1.0 mmol), Pd2(dba)3 (0.078 g, 0.087 mmol), XantPhos (0.096 g, 0.17 mmol), Cs2CO3 (0.57 g, 1.7 mmol) and dioxane (5 mL). The mixture was degassed with N2 for 10 min. The resulting mixture was irradiated in a microwave reactor at 140 C. for 3 hours and then cooled to room temperature. The mixture was filtered through Celite and concentrated under reduced pressure. The residue was dissolved in DMF and purified by prep-HPLC (Gilson GX 281, Shim-pack PRC-ODS 250 mm×20 mm×2, gradient: CH3CN/10 mm/L NH4HCO3, 17 min) to give the desired product as a yellow solid (26 mg, yield: 9%). 1H NMR (500 MHz, DMSO-d6): delta 11.2 (s, 1H), 8.28 (s, 1H), 8.17 (d, J=5.5 Hz, 1H), 7.71 (s, 1H), 7.59 (d, J=7.5 Hz, 2H), 7.52 (t, J=3.5 Hz, 1H), 7.41 (m, 1H), 7.03 (s, 1H). LC-MS (ESI) m/z: 349.0 [M+H+].

Reference： [1]Patent: US2010/317643,2010,A1 .Location in patent: Page/Page column 97; 98

4
[ 1190380-49-4 ]
[ 1258298-00-8 ]
2,6-dichloro-N-(2-(1-(tetrahydro-2H-pyran-4-yl)-1H-pyrazol-4-ylamino)pyridin-4-yl)benzamide [ No CAS ]

Yield	Reaction Conditions	Operation in experiment
25%	With caesium carbonate;tris-(dibenzylideneacetone)dipalladium(0); 4,5-bis(diphenylphos4,5-bis(diphenylphosphino)-9,9-dimethylxanthenephino)-9,9-dimethylxanthene; In 1,4-dioxane; at 140℃; for 3.0h;Microwave irradiation; Inert atmosphere;	To a microwave tube was added N-(2-bromopyridin-4-yl)-2,6-dichlorobenzamide (0.083 g, 0.24 mmol), <strong>[1190380-49-4]1-(tetrahydro-2H-pyran-4-yl)-1H-pyrazol-4-amine</strong> (0.048 g, 0.29 mmol), Pd2(dba)3 (0.022 g, 0.024 mmol), XantPhos (0.028 g, 0.048 mmol), Cs2CO3 (0.16 g, 0.48 mmol) and dioxane (2 mL). The mixture was degassed with N2 for 10 min. The resulting mixture was irradiated in a microwave reactor at 140 C. for 3 hours and then cooled to room temperature. The mixture was filtered through Celite and concentrated under reduced pressure. The residue was dissolved in DMF and purified by prep-HPLC (Gilson GX 281, Shim-pack PRC-ODS 250 mm×20 mm×2, gradient: CH3CN/10 mm/L NH4HCO3, 17 min) to give the desired product as a white solid (26 mg, yield: 25%). 1H NMR (500 MHz, d6-DMSO): delta 10.87 (s, 1H), 8.83 (s, 1H), 8.02 (d, J=5.5 Hz, 1H), 7.97 (s, 1H), 7.60 (d, J=3.0 Hz, 2H), 7.53 (t, J=3 Hz, 1H), 7.43 (s, 1H), 7.24 (s, 1H), 6.77 (d, J=5.0 Hz, 1H), 4.34 (m, 1H), 3.98-3.94 (m, 2H), 3.49-3.45 (m, 2H), 1.95-1.91 (m, 4H). LCMS (ESI) m/z: 432.0 [M+H+].

Reference： [1]Patent: US2010/317643,2010,A1 .Location in patent: Page/Page column 98

5
[ 1258298-00-8 ]
[ 21717-95-3 ]
[ 1258294-07-3 ]

Yield	Reaction Conditions	Operation in experiment
45%	With caesium carbonate;tris-(dibenzylideneacetone)dipalladium(0); 4,5-bis(diphenylphos4,5-bis(diphenylphosphino)-9,9-dimethylxanthenephino)-9,9-dimethylxanthene; In 1,4-dioxane; at 130℃; for 0.5h;Microwave irradiation; Inert atmosphere;	A 25 mL microwave tube containing N-(2-bromopyridin-4-yl)-2,6-dichlorobenzamide (100 mg, 0.29 mmol), <strong>[21717-95-3]3-fluoropyridin-2-amine</strong> (42 mg, 0.38 mmol), Pd2(dba)3 (8 mg, 0.008 mmol), Cs2CO3 (190 mg, 0.58 mmol), 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene (Xantphos, 4 mg, 0.003 mmol), and dioxane (15 mL) was degassed and then charged by N2 (3×). The resulting mixture was then irradiated in a microwave reactor at 130 C. for 30 min. The mixture was diluted with dioxane (20 mL) and filtered through Celite. The filtrate was concentrated under reduced pressure and the residue was purified by reverse-phase HPLC (Gemini, 200 mm×25 mm, gradient: CH3CN/0.05% NH3.H2O, 50-80%, 10 min) to afford the desired product (377 mg, yield: 45%). 1H NMR (400 MHz, DMSO) delta 11.07 (s, 1H), 8.98 (s, 1H), 8.28-8.01 (m, 3H), 7.70-7.48 (m, 4H), 7.37 (s, 1H), 7.01 (s, 1H). LCMS (ESI) m/z: 378.5 [M+H+].

Reference： [1]Patent: US2010/317643,2010,A1 .Location in patent: Page/Page column 99; 100

6
[ 1258298-00-8 ]
[ 81428-99-1 ]
[ 1258294-16-4 ]
[ 1258294-14-2 ]
[ 1258294-13-1 ]
[ 1258294-15-3 ]

Yield	Reaction Conditions	Operation in experiment
	With caesium carbonate In 1,4-dioxane at 160℃; for 2h; Microwave irradiation; Inert atmosphere;	239.2 To a microwave tube was added N-(2-bromopyridin-4-yl)-2,6-dichlorobenzamide (50 mg, 0.15 mmol), 2-methylcyclopropanecarboxamide (15 mg, 0.15 mmol), Pd2(dba)3 (21 mg, 0.020 mmol), XantPhos (12 mg, 0.020 mmol), Cs2CO3 (147 mg, 0.45 mmol) and dioxane (3 mL).The mixture was degassed with N2 for 10 min. The resulting mixture was irradiated in a microwave reactor at 160° C. for 2 hours and then cooled to room temperature. The mixture was filtered through Celite and concentrated under reduced pressure. The residue was dissolved in DMF and purified by preparative HPLC (Gilson GX 281, Shim-pack PRC-ODS 250 mm×20 mm×2, gradient: CH3CN/10 mm/L NH4HCO3, 17 min) to give the desired product (20 mg, 38% yield) as a mixture of 4 stereoisomers. These enantiomers could be separated as described below.A mixture of four enantiomers (220 mg) was separated via chiral prep-HPLC (AD-H column, mobile phase: n-hexane/ethanol (0.1% DEA)=90:10) to give the first eluting peak (50 mg), which was assigned as trans-configuration via NOE. >99% ee (12.78 min, AS-H column, n-hexane/ethanol (0.1% DEA)=90:10, 25 min) 1H-NMR (500 MHz, MeOH-d4): δ 8.30 (s, 1H), 8.24 (d, J=6.0 Hz, 1H), 7.60 (d, J=6.05 Hz, 1H), 7.49-7.43 (m, 4H), 1.62 (m, 1H), 1.41 (m, 1H), 1.16 (d, J=6.5 Hz, 3H), 1.15 (m, 1H), 0.72 (m, 1H). LCMS (ESI) m/z: 364.1 [M+H+].The remaining steroisomers was separated via chiral prep-HPLC (AS-H column, mobile phase: n-hexane/ethanol (0.1% DEA)=90:10) to give the three remaining enantiomers.First eluting peak, 25 mg, which was assigned as trans-configuration via NOE. >99% ee (10.13 min, AS-H column, n-hexane/ethanol (0.1% DEA)=90:10, 25 min) 1H-NMR (500 MHz, MeOHd4): δ 8.32 (s, 1H), 8.24 (d, J=5.5 Hz, 1H), 7.60 (d, J=5.5 Hz, 1H,), 7.50-7.45 (m, 4H), 1.93 (m, 1H), 1.36 (m, 1H), 1.20 (d, J=6.5 Hz, 3H), 1.03 (m, 1H), 0.95 (m, 1H). LCMS (ESI) m/z: 364.1 [M+H+].Second eluting peak, 30 mg, which was assigned as cis-configuration via NOE. >99% ee (13.17 min, AS-H column, n-hexane/ethanol (0.1% DEA)=90:10, 25 min) 1H-NMR (500 MHz, MeOH-d4): δ 8.32 (s, 1H), 8.24 (d, J=5.5 Hz, 1H), 7.60 (d, J=5.5 Hz, 1H,), 7.50-7.45 (m, 4H), 1.93 (m, 1H), 1.36 (m, 1H), 1.20 (d, J=6.5 Hz, 3H), 1.03 (m, 1H), 0.95 (m, 1H). LCMS (ESI) m/z: 364.1 [M+H+].Third eluting peak, 35 mg, which was assigned as cis-configuration via NOE. >99% ee (18.61 min, AS-H column, n-hexane/ethanol (0.1% DEA)=90:10, 25 min) 1H-NMR (500 MHz, MeOH-d4): δ 8.30 (s, 1H), 8.24 (d, J=6.0 Hz, 1H), 7.60 (d, J=6.05 Hz, 1H), 7.49-7.43 (m, 4H), 1.62 (m, 1H), 1.41 (m, 1H), 1.16 (d, J=6.5 Hz, 3H), 1.15 (m, 1H), 0.72 (m, 1H). LCMS (ESI) m/z: 364.1 [M+H+].

Reference： [1]Current Patent Assignee: ROCHE HOLDING AG - US2010/317643, 2010, A1 Location in patent: Page/Page column 103

7
[ 1258298-00-8 ]
[ 94-09-7 ]
[ 1258292-78-2 ]

Yield	Reaction Conditions	Operation in experiment
80%	With caesium carbonate In 1,4-dioxane at 120℃; for 0.5h; Microwave irradiation; Inert atmosphere;	234.1 A 25 mL microwave tube containing N-(2-bromopyridin-4-yl)-2,6-dichlorobenzamide (0.50 g, 1.40 mmol), ethyl 4-aminobenzoate (0.31 g, 1.92 mmol), Pd2(dba)3 (40 mg, 0.043 mmol), Cs2CO3 (0.94 g, 2.91 mmol), 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene (Xantphos, 17 mg, 0.029 mmol), and dioxane (20 mL) was degassed and then charged by N2 (3×). The mixture was then heated at 120° C. for 30 min and then diluted with dioxane (20 mL). The reaction was filtered through Celite and concentrated under reduced pressure. The residue was purified by reverse-phase HPLC (Gemini, 200 mm×25 mm, gradient: CH3CN/0.05% NH3.H2O, 50-80%, 10 min) to afford ethyl 4-(4-(2,6-dichlorobenzamido)pyridin-2-ylamino)benzoate (500 mg, yield: 80%). 1H NMR (400 MHz, DMSO) δ 11.02 (s, 1H), 9.60 (s, 1H), 8.15 (d, J=5.6, 1H), 7.96-7.76 (m, 4H), 7.57 (ddd, J=16.0, 9.0, 4.2, 4H), 6.92 (dd, J=5.6, 1.6, 1H), 4.27 (q, J=7.1, 2H), 1.31 (t, J=7.1, 3H). LCMS (ESI) m/z: 431.4 [M+H+].

Reference： [1]Current Patent Assignee: ROCHE HOLDING AG - US2010/317643, 2010, A1 Location in patent: Page/Page column 100

8
[ 4472-44-0 ]
[ 1258298-00-8 ]
[ 1258294-02-8 ]

Yield	Reaction Conditions	Operation in experiment
8%	With caesium carbonate;tris-(dibenzylideneacetone)dipalladium(0); 4,5-bis(diphenylphos4,5-bis(diphenylphosphino)-9,9-dimethylxanthenephino)-9,9-dimethylxanthene; In 1,4-dioxane; at 140℃; for 3h;Microwave irradiation; Inert atmosphere;	To a microwave tube was added N-(2-aminopyridin-4-yl)-2,6-dichlorobenzamide (0.25 g, 0.89 mmol), <strong>[4472-44-0]2-chloro-4,6-dimethylpyrimidine</strong> (0.19 g, 1.34 mmol), Pd2(dba)3 (0.81 g, 0.089 mmol), XantPhos (0.104 g, 0.179 mmol), Cs2CO3 (0.85 g, 2.6 mmol) and dioxane (4 mL). The mixture was degassed with N2 for 10 min. The resulting mixture was irradiated in a microwave reactor at 140° C. for 3 hours and then cooled to room temperature. The mixture was filtered through Celite and concentrated under reduced pressure. The residue was purified by column chromatography to afford the desired product as a white solid (22 mg, yield: 8percent). 1H NMR (500 MHz, MeOH-d4): delta 8.96 (d, J=1.5 Hz, 1H), 8.17 (d, J=5.5 Hz, 1H), 7.41-7.54 (m, 4H), 6.77 (s, 1H), 2.44 (s, 6H). LCMS (ESI) m/z: 388.0 [M+H+].

Reference： [1]Patent: US2010/317643,2010,A1 .Location in patent: Page/Page column 97

9
[ 1258298-00-8 ]
[ 81428-99-1 ]
[ 1258294-14-2 ]
[ 1258294-13-1 ]
C₁₇H₁₅Cl₂N₃O₂ [ No CAS ]

Yield	Reaction Conditions	Operation in experiment
	Multi-step reaction with 2 steps 1: tris-(dibenzylideneacetone)dipalladium⁽⁰⁾; 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene; caesium carbonate / 1,4-dioxane / 2 h / 160 °C / Inert atmosphere; Microwave irradiation 2: triethylamine / hexane; ethanol / Resolution of racemate

Reference： [1]Liang, Jun; Van Abbema, Anne; Balazs, Mercedesz; Barrett, Kathy; Berezhkovsky, Leo; Blair, Wade; Chang, Christine; Delarosa, Donnie; Devoss, Jason; Driscoll, Jim; Eigenbrot, Charles; Ghilardi, Nico; Gibbons, Paul; Halladay, Jason; Johnson, Adam; Kohli, Pawan Bir; Lai, Yingjie; Liu, Yanzhou; Lyssikatos, Joseph; Mantik, Priscilla; Menghrajani, Kapil; Murray, Jeremy; Peng, Ivan; Sambrone, Amy; Shia, Steven; Shin, Young; Smith, Jan; Sohn, Sue; Tsui, Vickie; Ultsch, Mark; Wu, Lawren C.; Xiao, Yisong; Yang, Wenqian; Young, Judy; Zhang, Birong; Zhu, Bing-Yan; Magnuson, Steven [Journal of Medicinal Chemistry, 2013, vol. 56, # 11, p. 4521 - 4536]

10
[ 1258298-00-8 ]
[ 81428-99-1 ]
[ 1258298-40-6 ]

Yield	Reaction Conditions	Operation in experiment
38%	With tris-(dibenzylideneacetone)dipalladium⁽⁰⁾; caesium carbonate; 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene In 1,4-dioxane at 160℃; for 2h; Inert atmosphere; Microwave irradiation;

11
[ 5469-70-5 ]
[ 1258298-00-8 ]
[ 1258293-25-2 ]

Yield	Reaction Conditions	Operation in experiment
	With palladium diacetate; caesium carbonate; 4,5-bis(diphenylphosphino)-9,9-dimethylxanthene In 1,4-dioxane at 150℃; for 0.333333h; Microwave irradiation; Inert atmosphere; Sealed tube;	6.2.10 2,6-Dichloro-N-(2-(pyrimidin-4-ylamino)pyridin-4-yl)benzamide (37) General procedure: A 20mL microwave tube was charged with pyrimidin-4-amine (220mg, 2.3mmol), N-(2-bromopyridin-4-yl)-2,6-dichloro benzamide (1.2g, 0.35mmol), Pd(OAc)2 (52mg, 0.23mmol), 4,5-bis(diphenylphosphino)-9,9-dimethylxantene (Xantphos, 0.27g, 0.46mmol), cesium carbonate (1.5g, 4.6mmol) and 1,4-dioxane (6mL). The mixture was degassed with nitrogen. The tube was sealed, and heated by microwave at 150°C for 20min. The mixture was purified by silica gel column chromatography (0-15% DCM/MeOH) to afford the desired product (70mg, 8.4% yield).

Reference： [1]Liang, Jun; Tsui, Vickie; Van Abbema, Anne; Bao, Liang; Barrett, Kathy; Beresini, Maureen; Berezhkovskiy, Leo; Blair, Wade S.; Chang, Christine; Driscoll, James; Eigenbrot, Charles; Ghilardi, Nico; Gibbons, Paul; Halladay, Jason; Johnson, Adam; Bir Kohli, Pawan; Lai, Yingjie; Liimatta, Marya; Mantik, Priscilla; Menghrajani, Kapil; Murray, Jeremy; Sambrone, Amy; Xiao, Yisong; Shia, Steven; Shin, Young; Smith, Jan; Sohn, Sue; Stanley, Mark; Ultsch, Mark; Zhang, Birong; Wu, Lawren C.; Magnuson, Steven [European Journal of Medicinal Chemistry, 2013, vol. 67, p. 175 - 187]

12
[ 876343-24-7 ]
[ 1258298-00-8 ]
[ 1258293-06-9 ]

Yield	Reaction Conditions	Operation in experiment
	With palladium diacetate; caesium carbonate; 4,5-bis(diphenylphos4,5-bis(diphenylphosphino)-9,9-dimethylxanthenephino)-9,9-dimethylxanthene; In 1,4-dioxane; at 150℃; for 0.333333h;Microwave irradiation; Inert atmosphere; Sealed tube;	General procedure: A 20mL microwave tube was charged with pyrimidin-4-amine (220mg, 2.3mmol), N-(2-bromopyridin-4-yl)-2,6-dichloro benzamide (1.2g, 0.35mmol), Pd(OAc)2 (52mg, 0.23mmol), 4,5-bis(diphenylphosphino)-9,9-dimethylxantene (Xantphos, 0.27g, 0.46mmol), cesium carbonate (1.5g, 4.6mmol) and 1,4-dioxane (6mL). The mixture was degassed with nitrogen. The tube was sealed, and heated by microwave at 150°C for 20min. The mixture was purified by silica gel column chromatography (0?15percent DCM/MeOH) to afford the desired product (70mg, 8.4percent yield).

Reference： [1]European Journal of Medicinal Chemistry,2013,vol. 67,p. 175 - 187

13
[ 1258298-00-8 ]
[ 1258292-64-6 ]

Yield	Reaction Conditions	Operation in experiment
	Multi-step reaction with 2 steps 1: tris-(dibenzylideneacetone)dipalladium⁽⁰⁾; DavePhos; lithium hexamethyldisilazane / tetrahydrofuran; 1,4-dioxane / 5 h / 100 °C / Microwave irradiation; Inert atmosphere; Sealed tube 2: pyridine / 4 h / 0 - 20 °C / Inert atmosphere

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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. 1258298-00-8 ] {[proInfo.proName]}

Quality Control of [ 1258298-00-8 ]

Related Doc. of [ 1258298-00-8 ]

Product Details of [ 1258298-00-8 ]

Safety of [ 1258298-00-8 ]

Application In Synthesis of [ 1258298-00-8 ]

[ 1258298-00-8 ] Synthesis Path-Downstream 1~13

Precautionary Statements-General

Prevention

Response

Storage

Disposal

Physical hazards

Health hazards

Environmental hazards

Inquiry