Hydrazine hydrate (1:1) → HCID 67713294, compound

HRID 1378074Notes

Reaction equation

HRID 1378074 reaction equation
O.[NH2:2][NH2:3].[F:4][C:5]1[CH:6]=[CH:7][C:8]2[N:14]3[CH:15]=[N:16][C:17]([C:18]([O-])=[O:19])=[C:13]3[CH2:12][N:11]([CH3:21])[C:10](=[O:22])[C:9]=2[CH:23]=1>C(O)C>[F:4][C:5]1[CH:6]=[CH:7][C:8]2[N:14]3[CH:15]=[N:16][C:17]([C:18]([NH:2][NH2:3])=[O:19])=[C:13]3[CH2:12][N:11]([CH3:21])[C:10](=[O:22])[C:9]=2[CH:23]=1

Participants

4

Reactant 2

HCID 24654Hydrazine hydrate (1:1)HCID 22914277HCID 22914277, compound

Product 1

HCID 67713294HCID 67713294, compoundYield 96%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

13 ml of hydrazine hydrate were added to a suspension of 7.0 g (23 mmol) of 8-fluoro-5-methyl-6-oxo-5,6-dihydro-4H-imidazo[1,5-a][1,4]benzodiazepin-3-carboxylate in 70 ml of ethanol and the mixture was heated at reflux for 3 hours. After cooling to 0° the crystals obtained were filtered off and there were obtained 6.43 g (96%) of 8-fluoro-5-methyl-6-oxo-5,6-dihydro-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxylic acid hydrazide as colourless needles of m.p. 288°-290°.

Workup

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

Sources & evidence

ORD record
ord-85f547da61894f89b1623438a5cdc79a
Source dataset
uspto-grants-1997_09
Patent number
US05665718

Reaction notes

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