Hydrazine hydrate (1:1) → HCID 85873980, compound

HRID 261553Notes

Reaction equation

HRID 261553 reaction equation
[C:1]([C:3]1[C:8]2[CH2:9][C:10](=O)[C:11]3[CH:17]=[CH:16][CH:15]=[CH:14][C:12]=3[S:13][C:7]=2[CH:6]=[CH:5][CH:4]=1)#[N:2].O.[NH2:20][NH2:21]>C(O)C>[C:1]([C:3]1[C:8]2[CH2:9][C:10](=[N:20][NH2:21])[C:11]3[CH:17]=[CH:16][CH:15]=[CH:14][C:12]=3[S:13][C:7]=2[CH:6]=[CH:5][CH:4]=1)#[N:2]

Participants

4

Reactant 2

HCID 24654Hydrazine hydrate (1:1)HCID 126870859-Cyano 10,11-dihydro-11-oxo-dibenzo[b,f]thiepin

Product 1

HCID 85873980HCID 85873980, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

g g. of 9-cyano-10,11-dihydro-11-oxo-dibenzo[b,f]thiepin and 1 g of 100 % hydrazine hydrate were dissolved in 10 ml of ethanol and the resulting mixture was heated under reflux for 3.5 hours. The reaction mixture was concentrated to 5 ml to separate crystals on cooling, which were collected by filtration. Recrystallization from ethanol afforded 0.6 g of 9-cyano-10,11-dihydro-11-oxo-dibenzo[b,f]thiepin hydrazone as pale brown prismatic crystals having a melting point of 175°-177° C.

Workup

  1. temperaturethe resulting mixture was heated
  2. temperatureunder reflux for 3.5 hours
  3. concentrationThe reaction mixture was concentrated to 5 ml
  4. customto separate crystals
  5. temperatureon cooling
  6. filtrationwhich were collected by filtration
  7. customRecrystallization from ethanol

Sources & evidence

ORD record
ord-ad8b8538cd45431094af931800e3bf08
Source dataset
uspto-grants-1979_08
Patent number
US04166127

Reaction notes

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