[ CAS No. 52667-88-6 ] {[proInfo.proName]}

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Quality Control of [ 52667-88-6 ]

COA NMR CNMR HPLC LC-MS

Related Doc. of [ 52667-88-6 ]

SDS Specification

Alternatived Products of [ 52667-88-6 ]

Product Details of [ 52667-88-6 ]

CAS No. :	52667-88-6	MDL No. :	MFCD00068689
Formula :	C₃₆H₄₄N₄O₈S₄	Boiling Point :	-
Linear Structure Formula :	-	InChI Key :	SKTWVKMQYXXWNY-UHFFFAOYSA-N
M.W :	789.02	Pubchem ID :	2802555
Synonyms :

Safety of [ 52667-88-6 ]

Signal Word:	Warning	Class:
Precautionary Statements:	P264-P280-P302+P352+P332+P313+P362+P364-P305+P351+P338+P337+P313	UN#:
Hazard Statements:	H315-H319	Packing Group:
GHS Pictogram:

Application In Synthesis of [ 52667-88-6 ]

* 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 [ 52667-88-6 ]
Downstream synthetic route of [ 52667-88-6 ]

[ 52667-88-6 ] Synthesis Path-Upstream 1~2

1
[ 52667-88-6 ]
[ 60239-18-1 ]

Reference： [1] Journal of Labelled Compounds and Radiopharmaceuticals, 2003, vol. 46, # 3, p. 197 - 209

2
[ 52667-88-6 ]
[ 175854-39-4 ]

Reference： [1] Research on Chemical Intermediates, 2012, vol. 38, # 8, p. 2085 - 2096
[2] Patent: JP2018/135304, 2018, A,

Yield	Reaction Conditions	Operation in experiment
55%		300 mL Place the rotor in a three-neck reaction vessel,200 mL isobaric dropping funnel, three way cock,Attach the balloon,The reaction vessel was shielded from light by an aluminum foil, immersed in an ice bath and dried under vacuum, and then 50 mL of dry DMF was added using a syringe while flowing nitrogen under a nitrogen-purged reaction vessel. further,1.69 g of NaH and 12.0 g (0.0212 mol) of N, N, N-tri (toluene-4-sulfonyl) diethylenetriamine were added in the order of nitrogen flow to the reaction vessel and stirred until no H 2 gas was evolved.The reaction vessel was transferred to an oil bath, the temperature was slowly raised to 70 C. and stirred at this temperature for 1 hour. after that,Slowly raise the oil bath temperature to 90 C,The mixture was stirred at this temperature for 1 hour.A solution of 12.0 g (0.0211 mol) of N, O, O-tri (tluene-4-sulfonyl) diethanolamine in 50 mL of dry DMF was placed in an equal pressure dropping funnel, and the mixture was slowly added dropwise and stirring was continued for 1 day. DMF was removed by distillation under reduced pressure,Distilled water was added to the remaining solid and cooled in a refrigerator. It was washed with distilled water, Et 2 0, EtOH and filtered, and hot filtered with MeOH to give a white solid(Yield 9.2402 g, 55%).

Yield	Reaction Conditions	Operation in experiment
1: 32% 2: 42%	In N,N-dimethyl-formamide at 50℃;

Yield	Reaction Conditions	Operation in experiment
66%	With hydrogenchloride; sulfuric acid; Amberlyst A₂₆ at 120℃; for 48h;
48%	Stage #1: cyclen tetratosylate With sulfuric acid at 150℃; for 1h; Stage #2: With hydrogenchloride In ethanol	1-9 1,4,7,10-tetraazacyclododecane tetrahydrochloride Put the rotor in a 1L eggplant flask, and use a reflux tube, a three-way cock,A balloon was attached and vacuum dried.Add 1,4,7,10-tetraazacyclododecane-1,4,7,10-tetratosylate (48.1 g, 61.0 mmol) and conc. H2SO4 (35 mL) to the reaction vessel.The mixture was stirred at 150 ° C for 1 hour. After returning to room temperature, EtOH (260 mL), It was slowly added dropwise in the order of Et2O (420 mL). The resulting gray precipitate was filtered through Nutche and the resulting solid was transferred to a 500 mL Meyer.Dissolved in the smallest amount of H2O. This was filtered through Celite, washed with a small amount of H2O, and the filtrate was collected and concentrated to obtain a black oily substance.To this was added 12 M HCl (50 mL) and EtOH (300 mL) and stirred to give a gray solid (9.41 g, Yield 48%).
	With hydrogenchloride; sulfuric acid 1.) 100 deg C, 48 h; Yield given. Multistep reaction;

Yield	Reaction Conditions	Operation in experiment
99.2%	With sulfuric acid In water for 0.0138889h; microwave irradiation;
25.0 g	With sulfuric acid at 100℃; for 48h;

Yield	Reaction Conditions	Operation in experiment
88%	With sulfuric acid at 165℃;
87%	Stage #1: cyclen tetratosylate With sulfuric acid at 100℃; for 0.05h; Microwave irradiation; Stage #2: With hydrogenchloride In water Stage #3: With sodium hydroxide In water
85%	With sulfuric acid at 100 - 105℃; Heating; 30-48 h;

Yield	Reaction Conditions	Operation in experiment
95%	With potassium carbonate In N,N-dimethyl-formamide

Yield	Reaction Conditions	Operation in experiment
78%	With potassium carbonate In N,N-dimethyl-formamide at 100℃; for 30h;
61%	With potassium carbonate In N,N-dimethyl-formamide at 30℃; for 72h;
48%	With potassium carbonate In N,N-dimethyl-formamide at 35℃; for 24h;	b Step b, In a 2L flask, 20 g of potassium carbonate, 30 g of compound 2, 31 g of 1,2-dibromoethane were added,Dimethyl carbonate (800mL) was reacted at 35°C for 24h, and then it was cooled to room temperature. The reaction mixture was collected by filtration, and concentrated under reduced pressure. The residue was recrystallized from 50mL of ethanol and filtered. The solid product was collected and dried by blowing air at 50°C. White compound 3 was obtained. The reaction formula is as follows:

Yield	Reaction Conditions	Operation in experiment
	With pyridine for 2h; Ambient temperature; Yield given. Yields of byproduct given. Title compound not separated from byproducts;

Yield	Reaction Conditions	Operation in experiment
95%	With potassium carbonate In acetonitrile for 144h; Heating;

Yield	Reaction Conditions	Operation in experiment
58%	With hydrogen bromide; acetic acid for 65h; Heating;

Yield	Reaction Conditions	Operation in experiment
	Multi-step reaction with 2 steps 1: 76 percent / sodium hydroxide / H₂O / 1.) 5 deg C, 1 hr., 2.) 3 hrs., r.t. 2: 90 percent / tetrabutylammonium iodide, sodium hydroxide (50 percent) / toluene; H₂O / 9 h / Heating

Yield	Reaction Conditions	Operation in experiment
	Multi-step reaction with 2 steps 1: 97 percent / Et₃N / acetonitrile / 5 h / 20 °C 2: 78 percent / K₂CO₃ / dimethylformamide / 30 h / 100 °C

Yield	Reaction Conditions	Operation in experiment
	Multi-step reaction with 3 steps 1: 70 percent / H₂SO₄ / 48 h / 100 °C 2: 94 percent / pyridine / 4 h / 20 °C 3: 76 percent / KOH; Na₂CO₃ / methanol / 45 - 65 °C

Yield	Reaction Conditions	Operation in experiment
	Multi-step reaction with 2 steps 1: 54 percent / 96percent aq. H₂SO₄ / 72 h / 110 °C 2: aq. LiOH / ethanol / 6 h / Heating

Yield	Reaction Conditions	Operation in experiment
	Multi-step reaction with 2 steps 1: 54 percent / 96percent aq. H₂SO₄ / 72 h / 110 °C 2: 60 percent / dimethylformamide / 2 h / 110 - 120 °C

Yield	Reaction Conditions	Operation in experiment
	Multi-step reaction with 2 steps 1: 54 percent / 96percent aq. H₂SO₄ / 72 h / 110 °C 2: aq. LiOH / ethanol / 6 h / Heating

Yield	Reaction Conditions	Operation in experiment
	Multi-step reaction with 2 steps 1: pyridine / 2 h / Ambient temperature 2: Na₂CO₃ / acetonitrile / 144 h / Heating

Yield	Reaction Conditions	Operation in experiment
	Multi-step reaction with 2 steps 1: 41 percent / benzene / 29 h / 70 °C 2: 95 percent / K₂CO₃ / dimethylformamide

Yield	Reaction Conditions	Operation in experiment
	Multi-step reaction with 3 steps 1: sulfuric acid / neat (no solvent) / 0.05 h / 100 °C / Microwave irradiation 2: triethylamine / chloroform / 28 h / 20 °C / Inert atmosphere 3: potassium carbonate / acetonitrile / 24 h / 80 °C / Inert atmosphere

Yield	Reaction Conditions	Operation in experiment
	Multi-step reaction with 3 steps 1: sulfuric acid / neat (no solvent) / 0.05 h / 100 °C / Microwave irradiation 2: triethylamine / chloroform / 28 h / 20 °C / Inert atmosphere 3: potassium carbonate / acetonitrile / 24 h / 80 °C / Inert atmosphere

Yield	Reaction Conditions	Operation in experiment
	Multi-step reaction with 3 steps 1: sulfuric acid / neat (no solvent) / 0.05 h / 100 °C / Microwave irradiation 2: triethylamine / chloroform / 28 h / 20 °C / Inert atmosphere 3: potassium carbonate / acetonitrile / 24 h / 80 °C / Inert atmosphere

Yield	Reaction Conditions	Operation in experiment
	Multi-step reaction with 3 steps 1: sulfuric acid / neat (no solvent) / 0.05 h / 100 °C / Microwave irradiation 2: triethylamine / chloroform / 28 h / 20 °C / Inert atmosphere 3: potassium carbonate / acetonitrile / 24 h / 80 °C / Inert atmosphere

Yield	Reaction Conditions	Operation in experiment
	Multi-step reaction with 4 steps 1: sulfuric acid / neat (no solvent) / 0.05 h / 100 °C / Microwave irradiation 2: triethylamine / chloroform / 28 h / 20 °C / Inert atmosphere 3: potassium carbonate / acetonitrile / 24 h / 80 °C / Inert atmosphere 4: hydrogen bromide / ethanol / 1 h / 0 - 50 °C / Inert atmosphere; Sonication

Yield	Reaction Conditions	Operation in experiment
	Multi-step reaction with 4 steps 1: sulfuric acid / neat (no solvent) / 0.05 h / 100 °C / Microwave irradiation 2: triethylamine / chloroform / 28 h / 20 °C / Inert atmosphere 3: potassium carbonate / acetonitrile / 24 h / 80 °C / Inert atmosphere 4: hydrogen bromide / ethanol / 1 h / 0 - 50 °C / Inert atmosphere; Sonication

Yield	Reaction Conditions	Operation in experiment
	Multi-step reaction with 4 steps 1: sulfuric acid / neat (no solvent) / 0.05 h / 100 °C / Microwave irradiation 2: triethylamine / chloroform / 28 h / 20 °C / Inert atmosphere 3: potassium carbonate / acetonitrile / 24 h / 80 °C / Inert atmosphere 4: hydrogen bromide / ethanol / 1 h / 0 - 50 °C / Inert atmosphere; Sonication

Yield	Reaction Conditions	Operation in experiment
	Multi-step reaction with 4 steps 1: sulfuric acid / neat (no solvent) / 0.05 h / 100 °C / Microwave irradiation 2: triethylamine / chloroform / 28 h / 20 °C / Inert atmosphere 3: potassium carbonate / acetonitrile / 24 h / 80 °C / Inert atmosphere 4: hydrogen bromide / ethanol / 1 h / 0 - 50 °C / Inert atmosphere; Sonication

Yield	Reaction Conditions	Operation in experiment
	Multi-step reaction with 3 steps 1.1: sulfuric acid 2.1: triethylamine / chloroform / 2.5 h / 0 °C / Inert atmosphere 2.2: 14 h / 0 °C / Inert atmosphere 3.1: potassium carbonate / acetonitrile / 12 h / 0 - 70 °C / Inert atmosphere

Yield	Reaction Conditions	Operation in experiment
	Multi-step reaction with 4 steps 1.1: sulfuric acid 2.1: triethylamine / chloroform / 2.5 h / 0 °C / Inert atmosphere 2.2: 14 h / 0 °C / Inert atmosphere 3.1: potassium carbonate / acetonitrile / 12 h / 0 - 70 °C / Inert atmosphere 4.1: trifluoroacetic acid / dichloromethane / 5 h / 20 °C

Yield	Reaction Conditions	Operation in experiment
	Multi-step reaction with 2 steps 1.1: sulfuric acid 2.1: triethylamine / chloroform / 2.5 h / 0 °C / Inert atmosphere 2.2: 14 h / 0 °C / Inert atmosphere

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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:
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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.
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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

Yield	Reaction Conditions	Operation in experiment
86%	With sodium hydroxide In water; toluene Heating; 8-10 h;
	With sodium hydroxide; tetra-(n-butyl)ammonium iodide In toluene for 10h; Heating; Yield given;
	With sodium hydride 1.) DMF, 2.) DMF, 110 deg C, 6 h; Multistep reaction;

7.2 g	With hydrogenchloride; sulfuric acid 1.) 100 deg C, 70 h;
	Stage #1: cyclen tetratosylate With sulfuric acid In water at 80℃; for 24h; Stage #2: With hydrogenchloride In water	c Step c, Into a 2L four-necked bottle, 1000 mL of water, 62 g of sulfuric acid, and 16 g of compound 3 were successively added, and the temperature was raised to 80°C.Should be 24 hours, cooled to room temperature, transferred to another reactor of equal size, added ethanol 65g, crystallized, discharged, centrifuged, collected solid product, put into a 2L reactor, then add water 220mL, activated carbon 2g, stirring After decoloration for 4 hours, the material was discharged, centrifuged, and the filtrate was collected. 25 g of hydrochloric acid was added to form a salt and crystallized. The material was discharged and centrifuged. The solid product was collected and dried in a drying oven at 50° C. to obtain a crude white compound 4. The reaction formula is as follows:

70%	With hydrogen bromide; acetic acid; phenol at 50℃; for 14h;
70%	With sulfuric acid at 100℃; for 39h;
70%	With sulfuric acid at 100℃; for 48h;
60%	With sulfuric acid at 130℃; for 72h;
60%	Stage #1: cyclen tetratosylate With sulfuric acid at 170℃; for 6h; Stage #2: With hydrogen bromide In water Stage #3: With sodium hydroxide for 24h;
59%	With sulfuric acid at 100℃; for 48h;
57%	With sulfuric acid at 160℃; for 0.5h; Inert atmosphere;	1.1.4 1,4,7,10-tetraazacyclododecane (cyclen) Put a rotor in a 200 mL recovery flask,9.24 g (0.01171 mol) of cyclen · 4Ts and 46 mL of H 2 SO 4 were added, a reflux pipe equipped with a three way cock and a balloon was attached, vacuum drying and nitrogen substitution were carried out.The reaction vessel was immersed in an oil bath,Slowly raise the temperature to 160 ° C,The mixture was stirred at this temperature for 30 minutes. after that,Remove the oil bath, cool down to room temperature, remove the reflux tube, attach a 200 mL pressure equalizing dropping funnel,50 mL of EtOH was slowly added dropwise.Next, when 80 mL of Et 2 O was dropped slightly earlier, a dark brown solid precipitated, which was filtered and washed with EtOH and Et 2 O. This solid was dissolved in distilled water, filtered through celite, and the filtrate was concentrated with an evaporator to obtain a dark brown oily substance.When HCl and EtOH were added to the solution, a solid precipitated, which was washed and filtered with EtOH to obtain a pale brown solid of the desired hydrochloride(Yield 1.564 g, 42%).1.500 g (4.777 mmol) of this cyclen · 4 HCl was applied to an ion exchange column,The basic fractions were collected and concentrated to give a white solid.When CHCl 3 was added to this, impurities precipitated, so they were removed and again concentrated to obtain a white solid(Yield 0.4649 g, 57%).
54%	With sulfuric acid at 110℃; for 72h;
33%	With sulfuric acid at 115℃; for 28h;
	With sulfuric acid
	With sulfuric acid	a) Richman and Atkins Procedure This is one of the most commonly used methods for the synthesis of cyclen, consisting of multistep protection-deprotection strategy.5-7 The key step of this method involves reaction of a preformed salt of a tritosylamide with sulfonate esters as leaving group in N,N-Dimethylformamide (DMF). Final separation of cyclen needs severe conditions to remove the tosyl protecting groups. For this purpose, 97% H2SO4 is used. This is a useful method provided that care is taken in the useof pure and dry starting materials. It has been reported to produce cyclen with a high yield (more than 60 %).

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

Yield	Reaction Conditions	Operation in experiment
	Multi-step reaction with 2 steps 1: 97 percent / Et₃N / acetonitrile / 5 h / 20 °C 2: 78 percent / K₂CO₃ / dimethylformamide / 30 h / 100 °C
	Multi-step reaction with 2 steps 1: 78.6 percent / aq. NaOH / diethyl ether / 1 h / Ambient temperature 2: 1.) NaOEt / 1.) EtOH, reflux, 30 min, 2.) DMF, 110 deg C, 24 h

Yield	Reaction Conditions	Operation in experiment
	Multi-step reaction with 2 steps 1.1: 58 percent / NaOH / diethyl ether; H₂O / 20 °C 2.1: NaH / dimethylformamide / 2 h 2.2: 86 percent / dimethylformamide / 2 h / Heating
	Multi-step reaction with 2 steps 1.1: 81 percent / Et₃N / CH₂Cl₂ / 0 - 20 °C 2.1: NaH / dimethylformamide / 2 h 2.2: 86 percent / dimethylformamide / 2 h / Heating

Yield	Reaction Conditions	Operation in experiment
	Multi-step reaction with 3 steps 1: 78 percent / 4 N NaOH / diisopropyl ether; H₂O / 1.) r.t., 15 h, 2.) pH 11, ca. 80 deg C, 30 min 2: 91 percent / sodium ethoxide / ethanol / 1 h / Heating 3: 67 percent / dimethylformamide / 1 h / Heating
	Multi-step reaction with 2 steps 1: 47 percent / pyridine / 4 h / 10 - 15 °C 2: 67 percent / dimethylformamide / 1 h / Heating
	Multi-step reaction with 2 steps 1: pyridine 2: sodium ethanolate / ethanol

	Multi-step reaction with 2 steps 1.1: sodium hydroxide / water; diethyl ether / 4 h 2.1: sodium hydride / N,N-dimethyl-formamide / 2 h / 70 - 90 °C / Inert atmosphere 2.2: 24 h
	Multi-step reaction with 2 steps 1.1: sodium hydroxide; N-benzyl-N,N,N-triethylammonium chloride / water; dichloromethane / 1 h 2.1: sodium hydride / N,N-dimethyl-formamide / 2 h / 70 - 90 °C / Inert atmosphere 2.2: 24 h
	Multi-step reaction with 2 steps 1.1: sodium hydroxide; N-benzyl-N,N,N-triethylammonium chloride / dichloromethane; water / 20 °C / Cooling with ice 2.1: sodium hydride / N,N-dimethyl-formamide; mineral oil / 1 h / 70 - 90 °C / Cooling with ice; Inert atmosphere 2.2: Inert atmosphere

Yield	Reaction Conditions	Operation in experiment
	Multi-step reaction with 2 steps 1: sulfuric acid / neat (no solvent) / 0.05 h / 100 °C / Microwave irradiation 2: triethylamine / chloroform / 28 h / 20 °C / Inert atmosphere
	Multi-step reaction with 2 steps 1: sulfuric acid / 0.5 h / 160 °C / Inert atmosphere 2: triethylamine / chloroform / 20 h / 0 - 20 °C
	Multi-step reaction with 3 steps 1: sulfuric acid / 1 h / 150 °C 2: hydrogenchloride 3: triethylamine / chloroform / 6 h / Cooling with ice

[ CAS No. 52667-88-6 ] {[proInfo.proName]}

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[ 52667-88-6 ] Synthesis Path-Upstream 1~2

[ 52667-88-6 ] Synthesis Path-Downstream 1~40

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