反应详情

To a solution of 5-cyclopropyl-3-phenyl-isoxazole-4-carboxylic acid methoxy-methyl-amide (4.00 g, 14.7 mmol) in THF (42 mL) cooled to −78° C. was added a solution of methylmagnesium bromide (3 M in diethylether, 9.80 mL, 29.4 mmol) dropwise within 5 min at −78° C. The cooling bath was removed and the reaction mixture was allowed to warm up to room temperature over 2.5 h. The reaction mixture was then re-cooled to −78° C., diluted with a saturated ammonium chloride solution (50 mL), allowed to warm up to room temperature and then diluted with water and extracted with ethyl acetate. The combined organic layers were then washed with brine and then dried over sodium sulphate and evaporated to afford the title compound (3.2 g, 94%) which was obtained as a light yellow solid. MS: m/e=228.3 [M+H]+.

1. customThe cooling bath was removed
2. temperatureThe reaction mixture was then re-cooled to −78° C.
3. additiondiluted with a saturated ammonium chloride solution (50 mL)
4. temperatureto warm up to room temperature
5. additiondiluted with water
6. extractionextracted with ethyl acetate
7. washThe combined organic layers were then washed with brine
8. dry with materialdried over sodium sulphate
9. customevaporated