反应详情

A solution of methyl 2-(2-benzyl-4-methyl-6-phenylpyrimidin-5-yl)pentanoate (67 mg; 0.17 mmol) in ethanol (1 mL), tetrahydrofuran (1 mL) and 2N sodium hydroxide solution (0.895 mL; 1.789 mmol) was stirred for 40 h at room temperature. The reaction mixture was concentrated under reduced pressure, diluted with water and acidified with a 6N hydrochloric acid solution. The suspension was extracted twice with ethyl acetate and the organic layers were washed with water and dried by filtration over a phase separater filter (PS1). The crude material was purified first by flash chromatography on silica gel using a linear gradient of methanol (1-10%) in dichloromethane and then by preparative thick layer chromatography on silica gel eluting with 10% methanol in dichloromethane to give 25 mg (37%) of the title compound as a colorless oil. ESI/APCI(+): 361 (M+H).

1. concentrationThe reaction mixture was concentrated under reduced pressure
2. additiondiluted with water
3. extractionThe suspension was extracted twice with ethyl acetate
4. washthe organic layers were washed with water
5. customdried by filtration over a phase separater
6. filtrationfilter (PS1)
7. customThe crude material was purified first by flash chromatography on silica gel using a linear gradient of methanol (1-10%) in dichloromethane