反应详情

温度

-78 °C

To a solution of N-methoxy-N-methyl-3-(2,2-dimethylpropyl)cyclobutanecarboxamide (95.2 g) in toluene (330 mL) was added diisobutylaluminum hydride (1.0M in toluene) (486 mL) dropwise at −78° C. After the mixture was stirred at −78° C. for 3 hr, 1.5 M sulfuric acid (648 mL) was added dropwise to the mixture at ice temperature. The mixture was extracted with toluene and the combined organic layer was washed with 1 M sulfuric acid, water and brine, then dried over sodium sulfate. The sodium sulfate was filtered off and the filtrate comprising the title compound was used in the next step.

1. extractionThe mixture was extracted with toluene
2. washthe combined organic layer was washed with 1 M sulfuric acid, water and brine
3. dry with materialdried over sodium sulfate
4. filtrationThe sodium sulfate was filtered off