反应详情

A solution of 6-(4-fluorophenyl)-2-methylthieno[2,3-d]pyrimidin-4(3H)-one (0.2 g, 0.77 mmol) and diisopropylethylamine (0.26 ml, 1.54 mmol) in POCl3 (4 ml) was stirred under N2 at 90° C. for 3.5 hours. The reaction mixture was allowed to cool down to room temperature and poured into an ice-bath. The aqueous phase was extracted with diethyl ether. The combined organic layers were washed with a half-saturated NaHCO3 solution and brine, dried over Na2SO4, and concentrated under reduced pressure. The crude residue was purified by silica gel chromatography (CH2Cl2/MeOH 50:1) to yield the title compound as a white solid (14 mg, 6%).

1. additionpoured into an ice-bath
2. extractionThe aqueous phase was extracted with diethyl ether
3. washThe combined organic layers were washed with a half-saturated NaHCO3 solution and brine
4. dry with materialdried over Na2SO4
5. concentrationconcentrated under reduced pressure
6. customThe crude residue was purified by silica gel chromatography (CH2Cl2/MeOH 50:1)