反应 #1178475

反应方程式

1-benzhydryl-3-ethylazetidin-3-ol

methyl iodide

sodium hydride

→

title compound

收率 52.0%

1-Benzhydryl-3-ethyl-3-methoxyazetidine

收率 52.0%

溶剂

DMF

反应条件

后处理

1. 1
   workup.ADDITIONThis 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 separated by filtration
6. 6
   浓缩the solvent was concentrated under reduced pressure
7. 7
   其他The obtained residue was purified by flash chromatography (Flash Chromatography System from Biotage AB, column size: 25S, ethyl acetate/n-hexane=1/9-4/6)

实验过程

To a DMF (50 mL) solution of 1-benzhydryl-3-ethylazetidin-3-ol (2.18 g, 8.15 mmol), methyl iodide (0.51 mL, 8.15 mmol) and 60% sodium hydride (0.65 g, 16.31 mmol) were added at 0° C. under a nitrogen stream, and the mixture was stirred for 1.5 hours at the same temperature. This 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 separated by filtration, and then the solvent was concentrated under reduced pressure. The obtained residue was purified by flash chromatography (Flash Chromatography System from Biotage AB, column size: 25S, ethyl acetate/n-hexane=1/9-4/6), to obtain the title compound (1.18 g, 52%) as an oily matter.

来源