反应 #54919

ord-e790afca29034886892401cfb6b13f60

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度cooled in an ice bath
  2. 2
    workup.STIRRINGthe reaction mixture was stirred at room temperature for about 30 minutes
  3. 3
    其他The solid was collected
  4. 4
    洗涤washed with additional ethyl ether

实验过程

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.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US04151166uspto-grants-1979_04