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

HRID 866920Notes

Reaction equation

HRID 866920 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

0.9g of 9-cyano-10,11-dihydro-11-oxo-dibenzo[b,f]thiepin and 1g of 100% hydrazine hydrate were dissolved in 10ml of ethanol and the resulting mixture was heated under reflux for 3.5 hours. The reaction mixutre was concentrated to 5ml to separate crystals on cooling, which were collected by filtration. Recrystallization from ethanol afforded 0.6g 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 mixutre was concentrated to 5ml
  4. customto separate crystals
  5. temperatureon cooling
  6. filtrationwhich were collected by filtration
  7. customRecrystallization from ethanol

Sources & evidence

ORD record
ord-55993361452048f09fbe6cc7496394a0
Source dataset
uspto-grants-1978_07
Patent number
US04101667

Reaction notes

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