反应详情

温度

0 °C

Under an argon atmosphere, in a 50-mL pear-shaped evaporating flask was weighed a solution of lanthanum chloride lithium chloride complex in THF (15.6 mL) and cooled to 0° C. To the solution was added dropwise a solution of isobutylmagnesium chloride in THF (3.5 mL) and stirred at 0° C. for 3 hours. A solution of tert-butyl 2-methyl-4-oxopiperidine-1-carboxylate (1 g) in THF (2.0 mL) was further added dropwise. The reaction solution was stirred at 0° C. for 1 hour, heated to 25° C., poured to hydrochloric acid and extracted with ethyl acetate. The organic layer was washed with water and a saturated sodium chloride solution and dried over anhydrous magnesium sulphate. The filtrate was concentrated and the resulting residue was purified by silica gel chromatography (hexane:ethyl acetate=9:1→3:1) to give the titled compound (450 mg) having the following physical properties.

1. customUnder an argon atmosphere, in a 50-mL pear-shaped evaporating flask was weighed
2. stirringThe reaction solution was stirred at 0° C. for 1 hour
3. temperatureheated to 25° C.
4. extractionextracted with ethyl acetate
5. washThe organic layer was washed with water
6. dry with materiala saturated sodium chloride solution and dried over anhydrous magnesium sulphate
7. concentrationThe filtrate was concentrated
8. customthe resulting residue was purified by silica gel chromatography (hexane:ethyl acetate=9:1→3:1)