反应详情

温度

0 °C

To a suspension of LiAlH4 (0.995 g, 26.2 mmol) in THF (40 mL) was added a solution of 5-((R)-α-methylbenzyl)-4,7-dioxo-5-azaspiro[2.4]heptane (3.0 g, 13.1 mmol) in THF (10 mL) at 0° C. The reaction mixture was stirred at 0° C. for 2 hrs, then warmed up to 50° C. and continued to stir for 6 hrs. The reaction mixture was then cooled to 0° C. and ethyl acetate (10 mL) and water (10 mL) were added. The suspension was filtered and the filtrate was concentrated in vacuo. The residue was purified by a silica gel column chromatography (1:3 (v/v) 2-butanol/n-hexane) to afford the title compound as colorless oil (2.4 g, 85%).

1. temperaturewarmed up to 50° C.
2. stirringto stir for 6 hrs
3. temperatureThe reaction mixture was then cooled to 0° C.
4. filtrationThe suspension was filtered
5. concentrationthe filtrate was concentrated in vacuo
6. customThe residue was purified by a silica gel column chromatography (1:3 (v/v) 2-butanol/n-hexane)