反应详情

A solution of 4-(1H-pyrazol-4-yl)-7-[2-(trimethylsilyl)ethoxy]methyl-7H-pyrrolo[2,3-d]-pyrimidine (12.1 g, 0.0384 mol), 2-butenoic acid, 3-methyl-, ethyl ester (16.0 mL, 0.115 mol) and DBU (14.3 mL, 0.0959 mol) in ACN (100 mL) was heated at reflux for 3.5 hours. The solvent was removed in vacuo. The residue was diluted with water, extracted with ethyl acetate, and the combined organic extracts were washed with saturated ammonium chloride, dried over sodium sulfate, and concentrated. The crude residue was purified by flash column chromatography (ethyl acetate/hexanes) to yield the desired product (15.5 g, 91%).

1. temperatureat reflux for 3.5 hours
2. customThe solvent was removed in vacuo
3. additionThe residue was diluted with water
4. extractionextracted with ethyl acetate
5. washthe combined organic extracts were washed with saturated ammonium chloride
6. dry with materialdried over sodium sulfate
7. concentrationconcentrated
8. customThe crude residue was purified by flash column chromatography (ethyl acetate/hexanes)