反应 #1178469

反应方程式

1-Benzhydryl-3-(2-hydroxyethyl)azetidine

methyl iodide

sodium hydride

→

title compound

收率 42.1%

1-Benzhydryl-3-(2-methoxyethyl)azetidine

收率 42.1%

溶剂

DMF

反应条件

后处理

1. 1
   workup.STIRRINGThe reaction mixture was stirred for two hours at the same temperature
2. 2
   workup.ADDITIONpoured onto ice water
3. 3
   萃取the mixture was extracted with ethyl acetate
4. 4
   萃取The combined extract
5. 5
   洗涤was washed with ice water and saturated brine
6. 6
   干燥dried over anhydrous sodium sulfate
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: 40M, ethyl acetate:n-hexane=5:95)

实验过程

1-Benzhydryl-3-(2-hydroxyethyl)azetidine (1.58 g, 5.91 mmol) was suspended in DMF (30 mL), and under a nitrogen stream, methyl iodide (0.37 mL, 5.91 mmol) and 60% sodium hydride (355 mg, 8.87 mmol) were added at 0° C. with stirring. The reaction mixture was stirred for two hours at the same temperature and then poured onto ice water, and the mixture was extracted with ethyl acetate. The combined extract was washed with ice water and saturated brine, and dried over anhydrous sodium sulfate, 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: 40M, ethyl acetate:n-hexane=5:95), to obtain the title compound (700 mg, 42%) as an oily matter.

来源