93605-74-4|(1H-Imidazol-1-yl)(morpholino)methanone| Ambeed

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CAS No. :	93605-74-4
Formula :	C₈H₁₁N₃O₂
M.W :	181.19
SMILES Code :	O=C(N1CCOCC1)N2C=CN=C2
MDL No. :	MFCD00585304

GHS Pictogram:
Signal Word:	Warning
Hazard Statements:	H302-H312-H315-H319-H332-H335
Precautionary Statements:	P261-P264-P270-P271-P280-P301+P312-P302+P352-P304+P340-P305+P351+P338-P330-P332+P313-P337+P313-P362-P403+P233-P405-P501

Yield	Reaction Conditions	Operation in experiment
89.8%		In the reactor, add 230.0kg ethylenediamine,Under stirring, 93.0kg of N-phenoxycarbonylmorpholine was added, the temperature was raised to 64-70C, and the reaction was carried out for 6 hours.Recover ethylenediamine by distillation under reduced pressure, and when there is no liquid dripping,The temperature is controlled at 70±2C, and the vacuum distillation is continued for 1 hour.Reduce to room temperature, add 370.0kg of acetone, add 30% sodium hydroxide solution dropwise with stirring, adjust pH 11~12, precipitate a large amount of solids, filter, and concentrate the filtrate to recover acetone. Add 350.0 kg of water to the residue, stir to dissolve, control the temperature at 20C to 40C, add oxalic acid solids in batches to adjust to pH 2 to 3, and precipitate a small amount of solids. Spin filtration, concentrate the filtrate to a slurry state, add 600 kg of ethanol, reflux for 0.5 hours, and filter pressure to a crystallization tank. Cool down and crystallize, keep at 0~10C for 4 hours, filter, and dry the filter cake in a hot-air circulating oven at 50-60C for 8 hours to obtain almost white N-(2-aminoethyl)-4-morpholinecarboxamide oxalate The solid was 106.1kg, and the yield was 89.8%. HPLC purity: 99.97%, moisture: 0.7%, ethylenediamine: 0.02%, ethanol: 7ppm.
80.23%		Room temperature, Ethylenediamine (18.03 g) and 50 mL of dichloromethane were added to a 250 mL three-necked flask, Stir, A solution of 9.1 g of N-imidazole-4-morpholine formamide in dichloromethane (100 mL) was slowly added dropwise under constant pressure, Heating up to reflux, Reaction about 36h; After completion of the reaction, methylene chloride was distilled off at room temperature under reduced pressure, 65 C, Decompression to P ≤-0.07Mpa, The remaining ethylenediamine was distilled off, To no fractions, The remaining system was added to 20 mL of methanol, Continue at 65 C, Decompression to P ≤-0.07Mpa distillation, To no fractions, The remaining system was added to 20 mL of dichloromethane, Followed by distillation at 65 C under reduced pressure, To no fractions; Finally, 50mL of methanol dissolved, Ice bath temperature is less than 10 deg C, Slowly dropping oxalic acid in methanol solution, Until the pH value of 4 to 5 to stop dropping, filter, The filtrate was concentrated to no fractions, Ethyl acetate was added to 80 mL overnight, Precipitation of white solid, filter, Collecting filter cake, Dried in vacuo (35 C) to give 10.56 g of intermediate III, The yield was 80.23%;

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P337 + P313	IF eye irritation persists: Get medical advice/attention.
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Disposal
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P501	Dispose of contents/container to ...
P502	Refer to manufacturer/supplier for information on recovery/recycling

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CAS No.: 93605-74-4

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CAS No.: 93605-74-4

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[ 93605-74-4 ] Synthesis Path-Downstream 1~1

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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