反应详情

温度

90 °C

To a stirred solution of isopropylamine (123 mg, 2.08 mmol) in dioxane (5 mL) under argon and at room temperature was added trimethylaluminium (1.04 mL of a 2M solution in toluene, 2.08 mmol). After 1 h, a solution of 2-chloro-thiazole-5-carboxylic acid ethyl ester (100 mg, 0.522 mmol) in dioxane (5 mL) was added and the reaction mixture warmed to 90° C. After 6 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 30% ethyl acetate in heptane) gave the title compound (100 mg, 94%) as a white solid. MS: m/e=203.4 [M+H]+.

1. waitAfter 6 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 30% ethyl acetate in heptane)