反应详情

温度

0 °C

To a solution of 4-(4-dimethylaminophenylsulfanyl)-2-methylpent-2-enoic acid methyl ester (0.279 g, 1.0 mmol) in dry THF (4 mL) at 0° C. was added dropwise a solution of di-isobutylaluminium hydride in toluene (1M, 3.0 mL, 3.0 mmol), under an atmosphere of argon. After stirring at 0° C. for one hour (TLC monitoring), the mixture was quenched by addition of methanol (0.5 mL: CAUTION), then water (0.3 mL), 5% aqueous sodium hydroxide solution (0.3 mL) and lastly 30% aqueous sodium potassium tartrate (4 mL). The mixture was stirred for 2 hours at 20° C., then extracted with diethyl ether (3×10 mL). The combined organic layers were dried over anhydrous MgSO4, filtered and evaporated to give the title compound (0.22 g, 88%) as a colourless oil.

1. customthe mixture was quenched by addition of methanol (0.5 mL: CAUTION)
2. stirringThe mixture was stirred for 2 hours at 20° C.
3. extractionextracted with diethyl ether (3×10 mL)
4. dry with materialThe combined organic layers were dried over anhydrous MgSO4
5. filtrationfiltered
6. customevaporated