反应详情

温度

90 °C

To a stirred solution of isopropylamine (66 mg, 1.12 mmol) in dioxane (5 mL) under argon and at room temperature was added trimethylaluminium (0.60 mL of a 2M solution in toluene, 1.20 mmol). After 1 h, a solution of 2-(5-methyl-3-phenyl-isoxazol-4-ylmethoxy)-thiazole-5-carboxylic acid ethyl ester (100 mg, 0.28 mmol) in dioxane (5 mL) was added and the reaction mixture warmed to 90° C. After 3 h, the reaction mixture was cooled, quenched with Seignettes's salt solution and water, then extracted with dichloromethane. The combined organic extracts were dried, filtered and concentrated. Purification by chromatography (silica, 0 to 3% methanol in dichloromethane) gave the title compound (68 mg, 69%) as a white solid. MS: m/e=358.1 [M+H]+.

1. waitAfter 3 h
2. temperaturethe reaction mixture was cooled
3. customquenched with Seignettes's salt solution and water
4. extractionextracted with dichloromethane
5. customThe combined organic extracts were dried
6. filtrationfiltered
7. concentrationconcentrated
8. customPurification by chromatography (silica, 0 to 3% methanol in dichloromethane)