反应详情

温度

0 °C

A mixture of compound 3 (0.800 g, 2.905 mmol) in THF (25 mL) was stirred at 0° C. and was treated with solid lithium aluminum hydride (0.4352 g, 11.62 mmol). The mixture was brought to room temperature at which point it was heated to reflux for 1 hour. The reaction was quenched with H2O (1 mL), 3N NaOH solution (1 mL) and an additional aliquot of H2O (1 mL). The solution was filtered over celite and was rinsed with diethyl ether. The concentrated crude product was subject to flash chromatography on silica gel 5% 2M NH3 methanol/CH2Cl2, which resulted in a dark brown viscous liquid, compound 4 (0.27 g, 36%).

1. customwas brought to room temperature at which point it
2. temperaturewas heated
3. temperatureto reflux for 1 hour
4. customThe reaction was quenched with H2O (1 mL), 3N NaOH solution (1 mL)
5. filtrationThe solution was filtered over celite
6. washwas rinsed with diethyl ether
7. concentrationThe concentrated crude product