反应 #1178474
ord-644f17aedce74d7fad738d794b62b014
反应方程式
反应条件
后处理
- 1过滤Then, the reaction liquor was filtered through celite
- 2萃取the filtrate was extracted with ethyl acetate
- 3洗涤The extract was washed with saturated brine
- 4干燥dried over anhydrous sodium sulfate
- 5其他Sodium sulfate was separated by filtration
- 6浓缩the solvent was concentrated under reduced pressure
- 7其他The obtained residue was purified by flash chromatography (Flash Chromatography System from Biotage AB, column size: 40M, ethyl acetate/n-hexane=1/9 to 6/4)
实验过程
To a tetrahydrofuran solution (10 mL) of 1-benzhydrylazetidin-3-one (3.23 g, 13.61 mmol), a 1M-tetrahydrofuran solution of ethylmagnesium bromide (13.61 mL, 27.22 mmol) was added at −78° C. under a nitrogen stream, and the mixture was allowed to warm to −10° C. over 5 hours. A saturated aqueous solution of sodium hydrogen carbonate (20 mL) was added to the reaction liquor, and the mixture was stirred for 15 minutes. Then, the reaction liquor was filtered through celite, and the filtrate was extracted with ethyl acetate. The extract was washed with saturated brine, and then dried over anhydrous sodium sulfate. Sodium sulfate was separated by filtration, and the solvent was concentrated under reduced pressure. The obtained residue was purified by flash chromatography (Flash Chromatography System from Biotage AB, column size: 40M, ethyl acetate/n-hexane=1/9 to 6/4), to obtain the title compound (2.18 g, 60%) as an oily matter.