Hydrazine hydrate (1:1) → HCID 53670505, compound

HRID 903641Notes

Reaction equation

HRID 903641 reaction equation
[C:1]([C:3]1[C:8]2[CH2:9][C:10](=O)[C:11]3[CH:17]=[CH:16][C:15]([F:18])=[CH:14][C:12]=3[S:13][C:7]=2[CH:6]=[CH:5][CH:4]=1)#[N:2].O.[NH2:21][NH2:22]>C(O)C>[C:1]([C:3]1[C:8]2[CH2:9][C:10](=[N:21][NH2:22])[C:11]3[CH:17]=[CH:16][C:15]([F:18])=[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 12687086HCID 12687086, compound

Product 1

HCID 53670505HCID 53670505, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

The mixture of 1.0 g of 9-cyano-3-fluoro-10,11-dihydrodibenzo[b,f]thiepin-11-one, 1.1 g of 100% hydrazine hydrate and 16 ml of ethanol was heated under reflux for 4.5 hours. The reaction mixture was concentrated to about one-fifth. After cooling, crystals was collected by filtration, there was obtained 9-cyano-3-fluoro-10,11-dihydrodibenzo[b,f]thiepin-11-one hydrazone having a melting point of 178°-179° C. in quantitative yield.

Workup

  1. temperaturewas heated
  2. temperatureunder reflux for 4.5 hours
  3. concentrationThe reaction mixture was concentrated to about one-fifth
  4. temperatureAfter cooling
  5. filtrationcrystals was collected by filtration

Sources & evidence

ORD record
ord-74270b2c63f44a3a8fc54e35cbc71026
Source dataset
uspto-grants-1980_10
Patent number
US04228284

Reaction notes

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