反应详情

To a solution of 5-{2-[2-Methoxy-4-(4-methyl-piperazin-1-yl)-phenylamino]-pyrimidin-4-yl}-1H-pyrrole-3-carboxylic acid ethyl ester (0.5 g, 1.14 mmol) in tetrahydrofuran (25 mL) and dimethylsulfoxide (5 mL) cooled in a ice-water bath, NaH (50 mg, 1.26 mmol) and methyl iodide (0.08 mL, 1.26 mmol) were added. The reaction was continued at room temperature for 12 h, tetrahydrofuran was removed under vacuo, then dichloromethane (25 mL) was added and the organic phase washed with water (25 mL). The aqueous fraction was extracted with dichloromethane (2×20 mL). The organic fractions were combined, dried over sodium sulfate, filtered, and concentered in vacuo. Purification by flash chromatography on silica gel (eluant: dichloromethane/methanol 95/5) provided 382 mg (74%) of the title compound as a pale yellow solid.

1. customtetrahydrofuran was removed under vacuo
2. additiondichloromethane (25 mL) was added
3. washthe organic phase washed with water (25 mL)
4. extractionThe aqueous fraction was extracted with dichloromethane (2×20 mL)
5. dry with materialdried over sodium sulfate
6. filtrationfiltered
7. customPurification by flash chromatography on silica gel (eluant: dichloromethane/methanol 95/5)