反应详情

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.

1. stirringThe reaction mixture was stirred for two hours at the same temperature
2. additionpoured onto ice water
3. extractionthe mixture was extracted with ethyl acetate
4. extractionThe combined extract
5. washwas washed with ice water and saturated brine
6. dry with materialdried over anhydrous sodium sulfate
7. concentrationthe solvent was concentrated under reduced pressure
8. customThe obtained residue was purified by flash chromatography (Flash Chromatography System from Biotage AB, column size: 40M, ethyl acetate:n-hexane=5:95)