反应详情

温度

-45 °C

A mechanically stirred suspension of lithium aluminum hydride (6.59 g, 0.165 mol) in ether (1 L) was cooled to -45° C. under nitrogen. A solution of the product from Step A (0.150 mol) in ether (150 mL) was added, maintaining the temperature below -35° C. When the addition was complete, the reaction was warmed to 5° C., then recooled to -45° C. A solution of potassium hydrogen sulfate (36.1 g, 0.265 mol) in water was slowly added, maintaining the temperature below -5° C. After quenching, the reaction was stirred at room temperature for 1 h. The mixture was filtered through Celite, the ether evaporated, and the remainder partitioned between ethyl acetate and 2% potassium hydrogen sulfate. After washing with saturated brine, drying over magnesium sulfate and solvent removal, the title compound was obtained.

1. temperaturemaintaining the temperature below -35° C
2. additionWhen the addition
3. temperaturethe reaction was warmed to 5° C.
4. customrecooled to -45° C
5. temperaturemaintaining the temperature below -5° C
6. customAfter quenching
7. filtrationThe mixture was filtered through Celite
8. customthe ether evaporated
9. customthe remainder partitioned between ethyl acetate and 2% potassium hydrogen sulfate
10. washAfter washing with saturated brine
11. dry with materialdrying over magnesium sulfate and solvent removal