反应详情

温度

-45 °C

The Weinreb amide of N-t-butoxycarbonylisoleucine, prepared above, (1.98 g, 7.2 mmol) was dissolved in anhydrous ether (10 ml) and cooled to -45° C. Lithium aluminium hydride (10 ml of a 1N solution in ether, 10 mmol) was then added keeping the temperature below -35° C., after addition the solution was then allowed to warm to 5° C. The solution was then cooled to -45° C. and sodium sulfate decahydrate (5.00 g) added and the cooling bath removed. After 1 hour the solution was filtered through celite and the solvent removed under reduced pressure to yield the aldehyde (1.47 g, 95%) as a colourless oil, which was immediately used in the next reaction as it racemises at room temperature.

1. customthe temperature below -35° C.
2. additionafter addition the solution
3. temperatureto warm to 5° C
4. temperatureThe solution was then cooled to -45° C.
5. customthe cooling bath removed
6. filtrationAfter 1 hour the solution was filtered through celite
7. customthe solvent removed under reduced pressure