反应 #1178472

反应方程式

1-benzhydrylazetidin-3-one

methylmagnesium iodide

sodium hydrogen carbonate

→

title compound

收率 104.0%

1-Benzhydryl-3-methylazetidin-3-ol

收率 104.0%

溶剂

tetrahydrofuran

反应条件

后处理

1. 1
   workup.STIRRINGthe mixture was stirred for 15 minutes
2. 2
   过滤Then, the reaction liquor was filtered through celite
3. 3
   萃取the filtrate was extracted with ethyl acetate
4. 4
   洗涤The extract was washed with saturated brine
5. 5
   干燥dried over anhydrous sodium sulfate
6. 6
   其他Sodium sulfate was separated by filtration
7. 7
   浓缩the solvent was concentrated under reduced pressure
8. 8
   其他The obtained residue was purified by flash chromatography (Flash Chromatography System from Biotage AB, column size: 40S, ethyl acetate/n-hexane=1/4 to ethyl acetate)

实验过程

To a tetrahydrofuran solution (10 mL) of 1-benzhydrylazetidin-3-one (530 mg, 1.94 mmol), methylmagnesium iodide (0.84 M ether solution) (4.62 mL, 3.88 mmol) was added at 0° C. under a nitrogen stream, and the mixture was stirred for one hour at the same temperature. 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: 40S, ethyl acetate/n-hexane=1/4 to ethyl acetate), to obtain the title compound (511 mg, quant.) as an oily matter.

来源