反应详情

A mixture of 4-(bromoacetyl)-5-methyl-3-phenylisoxazole (commercially available) (112 mg, 0.4 mmol) and 2-amino-3-methylpyridine (43 mg, 0.4 mmol) in ethanol (2.5 mL) was heated under reflux under argon for 5 h. The mixture was then poured onto water and extracted with ethyl acetate. The combined organic layers were then washed with water and brine, dried over sodium sulphate and evaporated to leave a yellow oil. Purification by chromatography (SiO2, heptane:ethyl acetate=100:0 to 25:75) afforded the title compound (46 mg, 40%) which was obtained as a colourless oil. MS: m/e=290.3 [M+H]+.

1. temperaturewas heated
2. temperatureunder reflux under argon for 5 h
3. additionThe mixture was then poured onto water
4. extractionextracted with ethyl acetate
5. washThe combined organic layers were then washed with water and brine
6. dry with materialdried over sodium sulphate
7. customevaporated
8. customto leave a yellow oil
9. customPurification by chromatography (SiO2, heptane:ethyl acetate=100:0 to 25:75)