反应 #1178473

反应方程式

1-benzhydryl-3-methylazetidin-3-ol

methyl iodide

sodium hydride

→

title compound

收率 29.2%

1-Benzhydryl-3-methoxy-3-methylazetidine

收率 29.2%

溶剂

DMF

反应条件

后处理

1. 1
   workup.ADDITIONThe reaction liquor was poured onto ice water
2. 2
   萃取the mixture was extracted with ethyl acetate
3. 3
   洗涤The extract was washed with ice water and saturated brine in this order
4. 4
   干燥dried over anhydrous sodium sulfate
5. 5
   其他Sodium sulfate was removed
6. 6
   浓缩the solvent was concentrated under reduced pressure
7. 7
   其他The obtained residue was purified by thin layer chromatography (ethyl acetate/n-hexane=10/1

实验过程

To a DMF (2 mL) solution of 1-benzhydryl-3-methylazetidin-3-ol (123 mg, 0.486 mmol), methyl iodide (33.2 μl, 0.534 mmol) and 60% sodium hydride (29 mg, 0.729 mmol) were added at 0° C. under a nitrogen stream, and the mixture was stirred for one hour at the same temperature. The reaction liquor was poured onto ice water, and the mixture was extracted with ethyl acetate. The extract was washed with ice water and saturated brine in this order, and then dried over anhydrous sodium sulfate. Sodium sulfate was removed, and then the solvent was concentrated under reduced pressure. The obtained residue was purified by thin layer chromatography (ethyl acetate/n-hexane=10/1, v/v), to obtain the title compound (38 mg, 29%) as an oily matter.

来源