Hydrazine hydrate (1:1) → HCID 67713662, compound

HRID 1378087Notes

Reaction equation

HRID 1378087 reaction equation
O.[NH2:2][NH2:3].[Cl:4][C:5]1[C:10]2[C:11](=[O:25])[N:12]([CH3:24])[CH2:13][C:14]3[N:15]([CH:16]=[N:17][C:18]=3[C:19]([O:21]CC)=O)[C:9]=2[CH:8]=[CH:7][C:6]=1[F:26]>C(O)C>[Cl:4][C:5]1[C:10]2[C:11](=[O:25])[N:12]([CH3:24])[CH2:13][C:14]3[N:15]([CH:16]=[N:17][C:18]=3[C:19]([NH:2][NH2:3])=[O:21])[C:9]=2[CH:8]=[CH:7][C:6]=1[F:26]

Participants

4

Reactant 2

HCID 24654Hydrazine hydrate (1:1)HCID 22914361HCID 22914361, compound

Product 1

HCID 67713662HCID 67713662, compoundYield 63%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

9.15 ml of hydrazine hydrate were added to a suspension of 5.47 g (0.00162 mol) of ethyl 7-chloro-8-fluoro-5-methyl-6-oxo-5,6-dihydro-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxylate in 55 ml of ethanol and the mixture was heated at reflux for 18 hours. After cooling to 0° the crystals obtained were filtered off and there were obtained 3.28 g (63%) of 7-chloro-8-fluoro-5-methyl-6-oxo-5,6-dihydro-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxylic acid hydrazide as white crystals; m.p. 308°-310°.

Workup

  1. temperaturethe mixture was heated
  2. temperatureat reflux for 18 hours
  3. temperatureAfter cooling to 0° the crystals
  4. customobtained
  5. filtrationwere filtered off

Sources & evidence

ORD record
ord-ef2c126ea7ef48d2b2af475a2cffaefc
Source dataset
uspto-grants-1997_09
Patent number
US05665718

Reaction notes

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