反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
Racemic 2-butyl-6,7-dichloro-2-cyclopentyl-2,3-dihydro-5-hydroxy-1H-inden-1-one (34.1 g, 0.1M) was stirred in dimethylformamide (100 ml) with K2CO3 (41.5 g, 0.3M) at 25° for 20 minutes. The mixture was cooled to 15°, and trifluoromethanesulfonyl chloride (19.4 g, 0.115M) was added at 15°-20° over 20 minutes. The mixture was then stirred at 25° for 30 minutes and poured into a liter of ice and water. The oil was extracted with diethyl ether (4×125 ml) and the combined organic extracts were thoroughly washed with water, dried over (MgSO4) and concentrated under vacuum to obtain the product as a viscous amber oil weighing 47.3 g. This product was used in the next step without further purification.
WORKUP
后处理
- temperatureThe mixture was cooled to 15°
- extractionThe oil was extracted with diethyl ether (4×125 ml)
- washthe combined organic extracts were thoroughly washed with water
- dry with materialdried over (MgSO4)
- concentrationconcentrated under vacuum