Water → HCID 21288004, 화합물
반응식
[CH2:1]([S:3][C:4]1[CH:9]=[CH:8][C:7]([N+:10]([O-])=O)=[CH:6][N:5]=1)[CH3:2].[Cl-].[NH4+].O>C(O)C>[NH2:10][C:7]1[CH:8]=[CH:9][C:4]([S:3][CH2:1][CH3:2])=[N:5][CH:6]=1참가 물질
5
실험 절차
A mixture of 5.0 g of 2-ethylthio-5-nitropyridine, 27 g of ammonium chloride, 54 ml of water, and 108 ml of ethanol is heated to 70°-80° C., and 16.2 g of reduced iron is added slowly with stirring. The mixture is stirred at the same temperature for 45 minutes. The hot reaction mixture is filtered, and the filtrate is concentrated. To the residue is added 50 ml of water, and the mixture is extracted with three 50-ml portions of chloroform. The combined extracts are washed with water, dried over magnesium sulfate and concentrated to give 3.7 g of crude 5-amino-2-ethylthiopyridine.
후처리
- temperatureis heated to 70°-80° C.
- stirringThe mixture is stirred at the same temperature for 45 minutes
- filtrationThe hot reaction mixture is filtered
- concentrationthe filtrate is concentrated
- additionTo the residue is added 50 ml of water
- extractionthe mixture is extracted with three 50-ml portions of chloroform
- washThe combined extracts are washed with water
- dry with materialdried over magnesium sulfate
- concentrationconcentrated
출처 및 근거
- ORD 기록
- ord-d7d91356f9ed48b4b134f007fa5fc333
- 출처 데이터셋
- uspto-grants-1988_10
- 특허 번호
- US04778796
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