Sodium Sulfate → 2-(3-Hydroxypropylthio)thiophene
반응식
[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]=1참가 물질
5
반응 조건
- 온도
- 0 °C
실험 절차
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%).
후처리
- 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
출처 및 근거
- ORD 기록
- ord-47bb9bbd83cf4d7b8090e65ff39cfc15
- 출처 데이터셋
- uspto-grants-1989_07
- 특허 번호
- US04847289
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