反应详情

温度

0 °C

Lithium aluminum hydride (1 M in THF, 5.3 ml, 5.3 mmol) was added to a solution of (3R)-tert-butyl 3-(methoxy(methyl)carbamoyl)-3,4-dihydroisoquinoline-2(1H)-carboxylate (1.7 g, 5.0 mmol theory) in ether (16 ml) stirring at 0° C. under nitrogen. After stirring at 0° C. for 1 h, the reaction was slowly quenched with water (0.40 ml). Sodium hydroxide (1N, 0.80 ml) followed by water (0.60 ml) were then added and the resultant gelatinous precipitate was filtered through Celite® rinsing with ether and THF. The filtrate was evaporated and the residue transferred to a separatory funnel with EtOAc. Washing with brine and drying with MgSO4 afforded crude product (1.3 g, 100% yield) which was used in the next step without further purification.

1. stirringAfter stirring at 0° C. for 1 h
2. customthe reaction was slowly quenched with water (0.40 ml)
3. additionwere then added
4. filtrationthe resultant gelatinous precipitate was filtered through Celite®
5. washrinsing with ether and THF
6. customThe filtrate was evaporated
7. customthe residue transferred to a separatory funnel with EtOAc
8. washWashing with brine
9. dry with materialdrying with MgSO4