反应详情

温度

45 °C

To a solution of (3R)-1-((1R,2R)-2-benzyloxycyclohex-1-yl)-2,5-dioxopyrrolidin-3-yl acetate (3a) in toluene (446 g, 0.151 mol) was added 10% Pd/C (6.3 g, 50 wt-% water wet), and the reaction vessel was flushed twice with H2. The reaction mixture was agitated at 18° C. under H2 (5 bar) for 8 hours and at 45° C. under H2 (5 bar) for 15.5 hours. The progress of the reaction was monitored by HPLC. The reaction mixture was filtered, the filtrate was washed with toluene and the filtrate was concentrated in vacuo to give 3-(R)-1-[(1R,2R)-2-hydroxycyclohexyl]-2,5-dioxopyrrolidin-3-yl acetate (4a) as a white hygroscopic foam (46.0 g).

1. customthe reaction vessel was flushed twice with H2
2. filtrationThe reaction mixture was filtered
3. washthe filtrate was washed with toluene
4. concentrationthe filtrate was concentrated in vacuo