反应详情

温度

-78 °C

To a solution of N-methoxy-N-methyl-3-(2-ethylbutyl)cyclobutanecarboxamide (13.2 g) in methylene chloride (35 mL) was added dropwise diisobutylaluminum hydride (1.0 M in methylene chloride)(76.0 mL) at −78° C. After stirring at −78° C. for 2.5 hr, 1 M sulfuric acid was added dropwise to the mixture. The mixture was stirred at ice temperature for 20 min. The organic layer was removed, and the aqueous layer was extracted with methylene chloride (15 mL×2). The combined organic layer was washed with 0.5 N sulfuric acid (50 mL×2), water (50 mL) 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. stirringThe mixture was stirred at ice temperature for 20 min
2. customThe organic layer was removed
3. extractionthe aqueous layer was extracted with methylene chloride (15 mL×2)
4. washThe combined organic layer was washed with 0.5 N sulfuric acid (50 mL×2), water (50 mL) and brine
5. dry with materialdried over sodium sulfate
6. filtrationThe sodium sulfate was filtered off