反应详情

To a stirred solution of 3-butyl-5-methyl-isoxazole-4-carboxylic acid ethyl ester (9.8 g, 46.3 mmol) in THF (100 mL) under argon and at 0° C. was added lithiumaluminiumhydride (2.03 g, 53.4 mmol) in five portions. After 1 h the reaction mixture was quenched dropwise with Seignette salt solution. The reaction mixture was filtered and the filtrate extracted with ethyl acetate. The combined organic extracts were washed with Seignette salt solution then dried, filtered and concentrated. Purification by chromatography (silica, heptane:ethyl acetate=100:0 to 4:6) afforded the title compound (7.5 g, 95%) as a yellow liquid. MS: m/e=170.3 [M+H]+.

1. customAfter 1 h the reaction mixture was quenched dropwise with Seignette salt solution
2. filtrationThe reaction mixture was filtered
3. extractionthe filtrate extracted with ethyl acetate
4. washThe combined organic extracts were washed with Seignette salt solution
5. customthen dried
6. filtrationfiltered
7. concentrationconcentrated
8. customPurification by chromatography (silica, heptane:ethyl acetate=100:0 to 4:6)