Hydrazine hydrate (1:1) → HCID 178503086, compound

HRID 1598521Notes

Reaction equation

HRID 1598521 reaction equation
O.[NH2:2][NH2:3].[CH3:4][S:5][C:6](SC)=[CH:7][C:8]([C:10]1[C:15]([Cl:16])=[CH:14][C:13]([C:17]([F:20])([F:19])[F:18])=[CH:12][C:11]=1[Cl:21])=O>C(O)C>[Cl:21][C:11]1[CH:12]=[C:13]([C:17]([F:20])([F:19])[F:18])[CH:14]=[C:15]([Cl:16])[C:10]=1[C:8]1[CH:7]=[C:6]([S:5][CH3:4])[NH:3][N:2]=1

Participants

4

Reactant 2

HCID 24654Hydrazine hydrate (1:1)HCID 18929408HCID 18929408, compound

Product 1

HCID 178503086HCID 178503086, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

Hydrazine monohydrate (0.51 ml) was added dropwise to a solution of 3.6 g of 3,3-bis[methylthio]-1-(2,6-dichloro-4-trifluoromethylphenyl)-2-propen-1-one (17) in 40 ml of ethanol at room temperature, and the mixture was stirred for 45 minutes and then refluxed for 4 hours. The reaction mixture was concentrated under reduced pressure to obtain a residue, which was purified by column chromatography on silica gel (eluent: ether/hexane=2/5) to afford 3.3 g of the desired compound in the form of white crystals.

Workup

  1. temperaturerefluxed for 4 hours
  2. concentrationThe reaction mixture was concentrated under reduced pressure
  3. customto obtain a residue, which
  4. customwas purified by column chromatography on silica gel (eluent: ether/hexane=2/5)

Sources & evidence

ORD record
ord-239f780dab1941d5a9eb70d43e65e4a7
Source dataset
uspto-grants-1998_04
Patent number
US05739083

Reaction notes

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