Reaktion #54919

ord-e790afca29034886892401cfb6b13f60

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturcooled in an ice bath
  2. 2
    workup.STIRRINGthe reaction mixture was stirred at room temperature for about 30 minutes
  3. 3
    SonstigeThe solid was collected
  4. 4
    Waschenwashed with additional ethyl ether

Vorschrift

A solution of 5.48 grams (0.02 mole) of 2-benzoyl-4-chlorophenylisothiocyanate in about 50 ml of ethyl ether was added dropwise to a solution containing 1.5 ml (0.028 mole) of methyl hydrazine (98%) in about 50 ml of ethyl ether cooled in an ice bath. Additional ethyl ether was added to facilitate stirring. Following addition of the isothiocyanate, the reaction mixture was stirred at room temperature for about 30 minutes. The solid was collected and washed with additional ethyl ether to yield 5.82 grams (91% yield) of N-(2-benzoyl-4-chlorophenyl)-methyl-hydrazinecarbothioamide as a white solid. The melting point was found to be 168.5°-170° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04151166uspto-grants-1979_04