反应详情

温度

80 °C

To a stirred solution of 3-isobutoxy-5-methyl-isoxazole (570 mg, 3.67 mmol) in AcOH (15 mL) and water (18 mL) at ambient temperature was added ICl (716 mg, 4.40 mmol) and the reaction mixture heated at 80° C. After 2 h the reaction mixture was cooled to room temperature. After 14 h, a solution of sodium sulfite (Na2SO3, 1 g) in water (15 mL) was added and the reaction mixture extracted into ethyl acetate (2×50 mL). The combined extracts were washed with water (3×30 ml) and brine then dried over sodium sulfate, filtered and concentrated. Purification by chromatography (silica, 0-10% ethyl acetate in heptane) gave the title compound (706 mg, 68%) as a colourless liquid.

1. temperatureAfter 2 h the reaction mixture was cooled to room temperature
2. extractionthe reaction mixture extracted into ethyl acetate (2×50 mL)
3. washThe combined extracts were washed with water (3×30 ml) and brine
4. dry with materialthen dried over sodium sulfate
5. filtrationfiltered
6. concentrationconcentrated
7. customPurification by chromatography (silica, 0-10% ethyl acetate in heptane)