Water → HCID 21288004、化合物
反応式
[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]=1参加物
5
実験手順
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.
後処理
- 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
出典と根拠
- ORDレコード
- ord-d7d91356f9ed48b4b134f007fa5fc333
- 出典データセット
- uspto-grants-1988_10
- 特許番号
- US04778796
反応ノート
読み込み中…