反应详情

3-(2,2-Dimethylpropyl)cyclobutanecarboxylic acid (75.2 g) and DMF (600 mL) were mixed. After an addition of N,O-dimethylhydroxylamine hydrochloride (51.7 g), triethylamine (92.4 mL), HOBt.H2O (81.2 g) and WSC.HCl (101.6 g) to the mixture, the mixture was stirred at RT overnight. Water was poured into the reaction and the mixture was extracted with ethyl acetate/hexane=1/1. The organic layer was washed with 1 N hydrochloric acid, water, aqueous 10 w/v % sodium carbonate and water, then dried over sodium sulfate. The sodium sulfate was filtered off and the filtrate was concentrated in vacuo to give the title compound (95.2 g) as a crude product.

1. extractionthe mixture was extracted with ethyl acetate/hexane=1/1
2. washThe organic layer was washed with 1 N hydrochloric acid, water, aqueous 10 w/v % sodium carbonate and water
3. dry with materialdried over sodium sulfate
4. filtrationThe sodium sulfate was filtered off
5. concentrationthe filtrate was concentrated in vacuo