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

HRID 26641

反応式

HRID 26641 の反応式
[C:1]([C:9]1[CH:14]=[C:13]([Cl:15])[CH:12]=[CH:11][C:10]=1[N:16]=[C:17]=[S:18])(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH3:19][NH:20][NH2:21].[N-]=C=S>C(OCC)C>[C:1]([C:9]1[CH:14]=[C:13]([Cl:15])[CH:12]=[CH:11][C:10]=1[NH:16][C:17]([N:20]([CH3:19])[NH2:21])=[S:18])(=[O:8])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

5

反応物 3

HCID 6061MethylhydrazineHCID 5200219Sbb012730HCID 178418790HCID 178418790、化合物

生成物 1

HCID 13972523N-(2-benzoyl-4-chlorophenyl)-methyl-hydrazinecarbothioamide収率 91%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒3 回

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.

後処理

  1. temperaturecooled in an ice bath
  2. stirringthe reaction mixture was stirred at room temperature for about 30 minutes
  3. customThe solid was collected
  4. washwashed with additional ethyl ether

出典と根拠

ORDレコード
ord-e790afca29034886892401cfb6b13f60
出典データセット
uspto-grants-1979_04
特許番号
US04151166

関連ノート

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