反应详情

Under argon gas, 7-[4-(4-chlorobenzoyl)benzyl]-5-methyl-2-methylthio-7H-pyrrolo[2, 3-d]pyrimidin-4(3H)-one (254 mg) was dissolved in anhydrous DME (10 ml)-anhydrous DMF (6 ml). Then, 60% sodium hydride-oil (26.4 mg) was added with ice-cooling and, after 30 minutes of agitation, methyl iodide (98 mg) was added. Then, at room temperature, the mixture was stirred for 2.5 hours. This reaction mixture was diluted with ethyl acetate, washed with saturated aqueous NaCl solution, and dried over anhydrous sodium sulfate. The solvent was then distilled off under reduced pressure and the residue was purified by flash column chromatography (chloroform) to provide the title compound (176 mg). 1H-NMR (CDCl3) δ: 2.39(3H,s), 2.56(3H,s), 3.56(3H,s), 5.29(2H,s), 6.47(1H,d,J=l.OHz), 7.29(2H,d,J=8.4Hz), 7.45(2H,d,J=8.4Hz), 7.73(4H,d,J=8.4Hz).

1. additionwas added
2. washwashed with saturated aqueous NaCl solution
3. dry with materialdried over anhydrous sodium sulfate
4. distillationThe solvent was then distilled off under reduced pressure
5. customthe residue was purified by flash column chromatography (chloroform)