反应详情

To a solution of (5-methyl-3-pyridin-2-yl-isoxazol-4-yl)-methanol (3.0 g, 16 mmol) in DCM (30 mL) at 0° C. was added thionyl chloride (3.75 g, 32 mmol) and the resulting mixture stirred for 1 h and then evaporated. After 1 h the reaction mixture was quenched with a solution of sodium hydrogen carbonate (1N, 15 mL) and extracted with ethyl acetate. The combined extracts were washed with water, dried over sodium sulfate, filtered and concentrated to give the title compound (3.2 g, 96%) as a light brown solid. MS: m/e=209.1 [M+H]+.

1. customevaporated
2. customAfter 1 h the reaction mixture was quenched with a solution of sodium hydrogen carbonate (1N, 15 mL)
3. extractionextracted with ethyl acetate
4. washThe combined extracts were washed with water
5. dry with materialdried over sodium sulfate
6. filtrationfiltered
7. concentrationconcentrated