Methanol → HCID 22768408, compound

HRID 867065Notes

Reaction equation

HRID 867065 reaction equation
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]=[C:10](OCC)[CH2:9][N:8]=[C:7]([C:15]3[CH:20]=[CH:19][C:18]([O:21][CH3:22])=[CH:17][CH:16]=3)[C:6]=2[CH:23]=1.CO.O.[NH2:27][NH2:28]>O>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]=[C:10]([NH:27][NH2:28])[CH2:9][N:8]=[C:7]([C:15]3[CH:20]=[CH:19][C:18]([O:21][CH3:22])=[CH:17][CH:16]=3)[C:6]=2[CH:23]=1

Participants

5

Reactant 3

HCID 887MethanolHCID 24654Hydrazine hydrate (1:1)HCID 20317277HCID 20317277, compound

Product 1

HCID 22768408HCID 22768408, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

To a solution of 0.11 part of 7-chloro-2-ethoxy-5-(4-methoxyphenyl)-3H-1,4-benzodiazepine in 5 parts by volume of methanol is added 0.2 part by volume of hydrazine hydrate (100%). The mixture is stirred at room temperature for 1.5 hours, and poured into 20 parts by volume of water. The mixture is extracted with chloroform. Chloroform layer is washed with water and dried over anhydrous sodium sulfate. The solvent is distilled off. Treatment of the residue with benzene gives 7-chloro-2-hydrazino-5-(4-methoxyphenyl)-3H-1,4-benzodiazepine as crystals melting at 213°-215° C.

Workup

  1. extractionThe mixture is extracted with chloroform
  2. washChloroform layer is washed with water
  3. dry with materialdried over anhydrous sodium sulfate
  4. distillationThe solvent is distilled off

Sources & evidence

ORD record
ord-8e727f3973534d8d961e98681634b12a
Source dataset
uspto-grants-1978_07
Patent number
US04102881

Reaction notes

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