Ammonia → HCID 20533061, compound

HRID 1758921Notes

Reaction equation

HRID 1758921 reaction equation
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]([CH2:12][CH2:13]Cl)[CH:10]([CH2:15]Cl)[CH2:9][N:8]=[C:7]([C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=3)[C:6]=2[CH:23]=1.[NH3:24]>CO.C(Cl)(Cl)Cl>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]3[CH2:12][CH2:13][NH:24][CH2:15][CH:10]3[CH2:9][N:8]=[C:7]([C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=3)[C:6]=2[CH:23]=1

Participants

5

Reactant 2

HCID 222AmmoniaHCID 20533044HCID 20533044, compound

Product 1

HCID 20533061HCID 20533061, compoundYield 59%

Reagents, catalysts & solvents 2

HCID 887MethanolSolventHCID 6212ChloroformSolvent

Procedure

10 g 7-chloro-1-(β-chlorethyl)-2-chlormethyl-5-phenyl-2,3-dihydro-1H-1,4-benzodiazepine were reacted in 200 ml methanol with 20 g ammonia gas in a gas autoclave for 16 hours at 90° to 95° C. After heating of the solution under vacuum, the reaction material is yielded in chloroform and washed with dilute aqueous sodium hydroxide solution. After drying and evaporating of the solvent under vacuum the resultive oily reaction product is dissolved in ether. From the concentrated solution, 5 g of 1,2,3,4,4a,5-hexahydro-9-chloro-7-phenyl-pyrazino[1,2-a]-[1,4]benzodiazepine having a melting point of 132°-135° C. are obtained by crystallization.

Workup

  1. temperatureAfter heating of the solution under vacuum
  2. washwashed with dilute aqueous sodium hydroxide solution
  3. customAfter drying
  4. customevaporating of the solvent under vacuum the resultive oily reaction product
  5. dissolutionis dissolved in ether

Sources & evidence

ORD record
ord-1d9cb5ae9f11447fb118503e91cf41d6
Source dataset
uspto-grants-1982_07
Patent number
US04338314

Reaction notes

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