反应详情

10.1 g of N-(4,6-dihydroxy-2-methylsulfanylpyrimidin-5-yl)-4-methoxy-3,5-dimethylbenzamide in 55 ml of phosphorus oxychloride were heated at 60° C. for 3 h. After cooling, the solid obtained was filtered off with suction and washed with methyl tert-butyl ether. The solid was then dissolved in a mixture of dichloromethane and tetrahydrofuran, washed with saturated aqueous sodium bicarbonate solution, dried and concentrated under reduced pressure. This gave 5.9 g of the title compound. LC/MS (Method LC1): Rt=1.24 min; m/z=318.08 [M+H]+

1. temperatureAfter cooling
2. customthe solid obtained
3. filtrationwas filtered off with suction
4. washwashed with methyl tert-butyl ether
5. dissolutionThe solid was then dissolved in a mixture of dichloromethane and tetrahydrofuran
6. washwashed with saturated aqueous sodium bicarbonate solution
7. customdried
8. concentrationconcentrated under reduced pressure