反应详情

温度

0 °C

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%).

1. temperatureThe mixture was refluxed for 2 hours
2. temperaturecooled to 0° C.
3. filtrationThe solid was filtered
4. washwashed with CHCl3
5. concentrationthe filtrate was concentrated
6. additionWater was added to the residue
7. extractionextracted with CHCl3
8. customDrying
9. customsolvent evaporation