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温度

0 °C

Under nitrogen atmosphere, tert-butyl (2-fluoroethyl)carbamate (I-286) (2 g, 20.1 mmol) was dissolved in N,N-dimethylformamide (50 ml), then sodium hydride (55%, w/w) (803 mg, 18.4 mmol) was added to the solution at 0° C., followed by stirring at 0° C. for 30 minutes. After 30 minutes, iodomethane (1.2 ml, 19.7 mmol) was added, followed by stirring at room temperature for 19 hours. Ethyl acetate was added to the reaction liquid, followed by washing with saturated brine. The organic layer was dried over anhydrous magnesium sulfate, then the solvent was evaporated away under reduced pressure. The resulting residue was purified by silica gel column chromatography (eluent, n-hexane:ethyl acetate=3:1, v/V) to obtain the entitled compound (970 mg, 45%) as a white crystal.

1. waitAfter 30 minutes
2. stirringby stirring at room temperature for 19 hours
3. washby washing with saturated brine
4. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
5. customthe solvent was evaporated away under reduced pressure
6. customThe resulting residue was purified by silica gel column chromatography (eluent, n-hexane