反应详情

温度

90 °C

To a stirred solution of isopropylamine (77 mg, 1.3 mmol) in dioxane (3 mL) under argon and at room temperature was added trimethylaluminium (0.65 mL of a 2M solution in toluene, 1.3 mmol). After 1 h, a solution of 2-[2-(3-butyl-5-methyl-isoxazol-4-yl)-ethyl]-4-methyl-thiazole-5-carboxylic acid (100 mg, 0.32 mmol) in dioxane (4 mL) was added and the reaction mixture heated at 90° C. overnight. The reaction mixture was then cooled, quenched with ice water and extracted with dichloromethane. The combined extracts were washed with Seignette's salt solution then dried, filtered, and concentrated. Purification by chromatography (silica, 0 to 5% methanol in dichloromethane) gave the title compound (50 mg, 44%) as a light yellow oil. MS: m/e=350.5 [M+H]+.

1. temperatureThe reaction mixture was then cooled
2. customquenched with ice water
3. extractionextracted with dichloromethane
4. washThe combined extracts were washed with Seignette's salt solution
5. customthen dried
6. filtrationfiltered
7. concentrationconcentrated
8. customPurification by chromatography (silica, 0 to 5% methanol in dichloromethane)