反応 #54919

反応方程式

2-benzoyl-4-chlorophenylisothiocyanate

methyl hydrazine

isothiocyanate

→

N-(2-benzoyl-4-chlorophenyl)-methyl-hydrazinecarbothioamide

収率 91.0%

溶媒

ethyl ether

ethyl ether

ethyl ether

反応条件

後処理

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
   その他The solid was collected
4. 4
   洗浄washed with additional ethyl ether

実験手順

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.

出典