反应详情

Mono-tert-butyl 3-[4-cyclopropyl-5-(3-isobutylcyclobutyl)isoxazol-3-yl]glutarate (2.83 g) and DMF (28 mL) were mixed. After an addition of 2-chloro-5-methylphenylamine (1.184 g), HOBt.H2O (1.28 g) and WSC.HCl (1.60 g) to the resultant solution, the mixture was stirred at RT for 2 days. To the reaction mixture was added saturated aqueous sodium bicarbonate, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated aqueous sodium bicarbonate, water and brine, then dried over sodium sulfate. The sodium sulfate was filtered off and the filtrate was concentrated in vacuo. The resultant residue was purified by silica gel column chromatography (Eluent: ethyl acetate/hexane=1/15→1/10→1/8) to give the title compound (1.241 g).

1. extractionthe mixture was extracted with ethyl acetate
2. washThe organic layer was washed with saturated aqueous sodium bicarbonate, water and brine
3. dry with materialdried over sodium sulfate
4. filtrationThe sodium sulfate was filtered off
5. concentrationthe filtrate was concentrated in vacuo
6. customThe resultant residue was purified by silica gel column chromatography (Eluent: ethyl acetate/hexane=1/15→1/10→1/8)