反应详情

温度

0 °C

To a solution of 3-hexyl-6-methyl-6-[3-(4H-1,2,4-triazol-3-yl)phenyl]-3-azabicyclo[3.1.0]hexan-2-one (Preparation 43, 220 mg, 0.65 mmol) in tetrahydrofuran (5 ml) at room temperature was added lithium aluminium hydride (1.3 ml, 1.30 mmol, 1.0M in THF) dropwise over a few minutes. The mixture was then heated under reflux for 2 hours and then cooled to 0° C. 2N sodium hydroxide (1.0 ml) was added cautiously followed by ethyl acetate (10 ml) and the mixture was stirred rapidly for 30 minutes, then filtered through celite. The filtrate was concentrated in vacuo and the residue was purified by silica column chromatography eluting with ethyl acetate:methanol:amnonia solution (0.880) (80:20:1) to afford the title compound (190 mg, 90%) as a colourless oil.

1. temperatureThe mixture was then heated
2. temperatureunder reflux for 2 hours
3. filtrationfiltered through celite
4. concentrationThe filtrate was concentrated in vacuo
5. customthe residue was purified by silica column chromatography
6. washeluting with ethyl acetate