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

HRID 26641

반응식

HRID 26641 반응식
[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

참가 물질

5

반응물 3

HCID 6061MethylhydrazineHCID 5200219Sbb012730HCID 178418790HCID 178418790, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 3283Diethyl Ether용매3회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-e790afca29034886892401cfb6b13f60
출처 데이터셋
uspto-grants-1979_04
특허 번호
US04151166

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