反应详情

Tert-butyl 4-hydroxypiperidine-1-carboxylate (2.47 g, 12.3 mmol) and potassium tert-butoxide (1.42 g, 12.7 mmol) were added to a THF (20 mL) solution of 2,4-dichloro-3-methylpyrimidine (1.60 g, 9.82 mmol), and the mixture was stirred for 2 hours. To the reaction solution, water was added, followed by extraction with ethyl acetate three times. The obtained organic layer was washed with saturated saline and dried over anhydrous sodium sulfate, and the solvent was distilled off under reduced pressure. The obtained residue was purified by silica gel column chromatography (hexane:ethyl acetate=80:20-60:40, V/V) to obtain the title compound as colorless oil (3.07 g, yield: 95%).

1. extractionfollowed by extraction with ethyl acetate three times
2. washThe obtained organic layer was washed with saturated saline
3. dry with materialdried over anhydrous sodium sulfate
4. distillationthe solvent was distilled off under reduced pressure
5. customThe obtained residue was purified by silica gel column chromatography (hexane:ethyl acetate=80:20-60:40, V/V)