Sodium Sulfate → 2-(3-Hydroxypropylthio)thiophene
反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[C:7]([CH2:10][CH2:11][S:12][C:13]1[S:17][CH:16]=[CH:15][CH:14]=1)(O)=[O:8].[O-]S([O-])(=O)=O.[Na+].[Na+]>C1COCC1>[OH:8][CH2:7][CH2:10][CH2:11][S:12][C:13]1[S:17][CH:16]=[CH:15][CH:14]=1参加物
5
反応条件
- 温度
- 0 °C
実験手順
To a suspension of lithium aluminum hydride (20.1 g, 0.53 mol) in THF (125 ml), cooled to 0° C. was added a solution of 5-(2-carboxyethylthio)thiophene (25.0 g, 0.13 mol) in THF (125 ml) dropwise. The mixture was refluxed for 2 hours, cooled to 0° C. and saturated Na2SO4 was added dropwise. The solid was filtered, washed with CHCl3 and the filtrate was concentrated. Water was added to the residue and extracted with CHCl3. Drying and solvent evaporation gave an oily, product (21.7 g, 96%).
後処理
- temperatureThe mixture was refluxed for 2 hours
- temperaturecooled to 0° C.
- filtrationThe solid was filtered
- washwashed with CHCl3
- concentrationthe filtrate was concentrated
- additionWater was added to the residue
- extractionextracted with CHCl3
- customDrying
- customsolvent evaporation
出典と根拠
- ORDレコード
- ord-47bb9bbd83cf4d7b8090e65ff39cfc15
- 出典データセット
- uspto-grants-1989_07
- 特許番号
- US04847289
反応ノート
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