Acetic Anhydride → HCID 178475132, compound

HRID 1075746Notes

Reaction equation

HRID 1075746 reaction equation
C(O[C:5](=[O:7])[CH3:6])(=O)C.[Cl:8][C:9]1[CH:10]=[CH:11][C:12]2[N:18]=[C:17]([NH:19][NH2:20])[CH2:16][N+:15]([O-:21])=[C:14]([C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)[C:13]=2[CH:28]=1>C(Cl)Cl>[C:5]([NH:20][NH:19][C:17]1[CH2:16][N+:15]([O-:21])=[C:14]([C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)[C:13]2[CH:28]=[C:9]([Cl:8])[CH:10]=[CH:11][C:12]=2[N:18]=1)(=[O:7])[CH3:6]

Participants

4

Reactant 2

HCID 7918Acetic AnhydrideHCID 178514336HCID 178514336, compound

Product 1

HCID 178475132HCID 178475132, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

1.5 ml. of acetic anhydride was added to a solution of 2.5 g. of 7-chloro-2-hydrazino-5-phenyl-3H-1,4-benzodiazepine 4-oxide in 50 ml. of methylene chloride. After stirring for 15 minutes at room temperature, the mixture was concentrated and crystallized by addition of ether to yield 2-(2-acetylhydrazino)-7-chloro-5-phenyl-3H-1,4-benzodiazepine 4-oxide, which after recrystallization from dimethylformamide, had a melting point of 272°-275° dec.

Workup

  1. concentrationthe mixture was concentrated
  2. customcrystallized by addition of ether

Sources & evidence

ORD record
ord-af73bce23eb04538a5a13a3b57fa1b01
Source dataset
uspto-grants-1976_05
Patent number
US03954728

Reaction notes

Loading…