反应详情

温度

70 °C

A solution of 2-[1-(2,3-dihydrobenzo[1,4]dioxin-2-ylmethyl)piperidin-3-yl]ethanol (0.1 g, 0.36 mmol) in THF (5 ml) was added NaH (79.0 mg, 1.79 mmol), which was previously washed with heptane. The reaction mixture was stirred at 70° C. for 1 h followed by a dropwise addition of a solution of iodomethane (0.034 ml, 0.54 mmol) in THF (1 ml). Stirring was continued for 1 h. Water was slowly added and the reaction mixture was extracted with DCM (3×20 ml). The combined organic phases were dried (Na2SO4), filtered and the filtrate was evaporated to give the title compound, which was purified by column chromatography (DCM/MeOH, 90:10).

1. washwas previously washed with heptane
2. stirringStirring
3. waitwas continued for 1 h
4. extractionthe reaction mixture was extracted with DCM (3×20 ml)
5. dry with materialThe combined organic phases were dried (Na2SO4)
6. filtrationfiltered
7. customthe filtrate was evaporated