反应详情

温度

0 °C

Lithium aluminum hydride (0.24 g; 6.4 mmole) was slurried in THF (20 mL) and cooled to 0° C. The suspension was treated with a solution of the carbamate from (c) above (1.1 g; 4.6 mmole) in THF (10 mL) and stirred for 2 hours at 0° C. The mixture was further cooled to -30° C. and a solution of NaHSO4 (0.6 g; 4.3 mmole) in H2O (5 mL) was cautiously added and then diluted with EtOAc (50 mL), and filtered through celite. The filtrate was dried over MgSo4, filtered, and concentrated in vacuo leaving a colorless liquid. Yield: 1.0 g (100%)

1. temperatureThe mixture was further cooled to -30° C.
2. filtrationfiltered through celite
3. customThe filtrate was dried over MgSo4
4. filtrationfiltered
5. concentrationconcentrated in vacuo
6. customleaving a colorless liquid