Methylhydrazine → HCID 18929398, compound

HRID 1598524Notes

Reaction equation

HRID 1598524 reaction equation
[CH3:1][NH: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[N:2]([CH3:1])[N:3]=[C:6]([S:5][CH3:4])[CH:7]=1

Participants

4

Reactant 2

HCID 6061MethylhydrazineHCID 18929408HCID 18929408, compound

Product 1

HCID 18929398HCID 18929398, compoundYield 33.9%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

Methylhydrazine (1.9 g) was added dropwise to a solution of 5.0 g of 3,3-bis[methylthio]-1-(2,6-dichloro-4-trifluoromethylphenyl)-2-propen-1-one (22) in 50 ml of ethanol at room temperature, followed by refluxing for 3 hours. The solvent was distilled off under reduced pressure to obtain a residue, which was purified by column chromatography on silica gel, giving 1.6 g of the desired compound in the form of a brown oil (yield 28.5%).

Workup

  1. temperatureby refluxing for 3 hours
  2. distillationThe solvent was distilled off under reduced pressure
  3. customto obtain a residue, which
  4. customwas purified by column chromatography on silica gel

Sources & evidence

ORD record
ord-1452c7b3ad224451bb27b372a3d33fc4
Source dataset
uspto-grants-1998_04
Patent number
US05739083

Reaction notes

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