Methylhydrazine → N,1-Dimethyl-N-phenylhydrazinethiocarboxamide
반응식
[CH3:1][N:2]([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)[C:3](Cl)=[S:4].[CH3:12][NH:13][NH2:14]>CCOCC>[CH3:12][N:13]([C:3]([N:2]([CH3:1])[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)=[S:4])[NH2:14]참가 물질
4
실험 절차
To a solution of N-methyl-N-phenylthiocarbamyl chloride (79.6 g, 0.43 mole) in 250 ml dry ether, a solution of 39.5 g (0.86 mole) methylhydrazine in 100 ml of dry ether was added dropwise with stirring below 10° C. The reaction temperature was allowed to increase to room temperature and the mixture was filtered. The filtrate was evaporated to low volume and diluted with about 300 ml hexane. After stirring for a few hours the hexane layer was decanted. The hexane immiscible layer was reevaporated to remove organic solvents, giving the desired product, (70.0 g) as a thick orange liquid.
후처리
- filtrationthe mixture was filtered
- customThe filtrate was evaporated to low volume
- additiondiluted with about 300 ml hexane
- stirringAfter stirring for a few hours the hexane layer
- customwas decanted
- customThe hexane immiscible layer was reevaporated
- customto remove organic solvents
출처 및 근거
- ORD 기록
- ord-f194c1d7cf394b3da3692c083f32c8af
- 출처 데이터셋
- uspto-grants-1981_08
- 특허 번호
- US04282031
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