反应详情

温度

0 °C

To a solution of 2-[3-methoxy-4-(4-methyl-imidazol-1-yl)-phenylamino]-thiazole-4-carboxylic acid ethyl ester (20 mg, 0.056 mmol) in dry THF (2 ml) at 0° C. was added methylmagnesium bromide (3M solution in THF, 93 μl, 0.279 mmol) added and stirred at 0° C. for 2 h. The reaction mixture was cautiously quenched with saturated aqueous ammonium chloride solution. The aqueous phase was extracted three times with diethyl ether, dried over Na2SO4, filtered and the solvents were evaporated. The residue was purified by silica gel chromatography using dichloromethane/methanol as eluent. The title compound was obtained as a light brown oil (14.4 mg, 75%). MS ISP (m/e): 345.1 (100) [(M+H)+].

1. additionadded
2. customThe reaction mixture was cautiously quenched with saturated aqueous ammonium chloride solution
3. extractionThe aqueous phase was extracted three times with diethyl ether
4. dry with materialdried over Na2SO4
5. filtrationfiltered
6. customthe solvents were evaporated
7. customThe residue was purified by silica gel chromatography