反应详情

温度

-78 °C

To a solution of N-methoxy-N-methyl-3-isobutylcyclobutanecarboxamide (77 g) in methylene chloride (235 mL) was added dropwise diisobutylaluminum hydride (1.0 M in methylene chloride) (473.2 mL) at −78° C. The mixture was stirred at −78° C. for 2 hr. After an addition of 1.5 M sulfuric acid (630 mL) at ice temperature, the mixture was extracted with methylene chloride. The combined organic layer was washed with 1.5 M sulfuric acid, water and brine, then dried over magnesium sulfate. The magnesium sulfate was filtered off and the filtrate comprising the title compound was used in the next step.

1. extractionthe mixture was extracted with methylene chloride
2. washThe combined organic layer was washed with 1.5 M sulfuric acid, water and brine
3. dry with materialdried over magnesium sulfate
4. filtrationThe magnesium sulfate was filtered off