反应详情

温度

100 °C

To a solution of tert-butyl 4-(2,4-dioxo-6-phenyl-1,4-dihydrothieno[3,2-d]pyrimidin-3(2H)-yl)piperidine-1-carboxylate (5 g; compound B50) and chloroacetonitrile (883 mg) in DMF (45 ml) is added potassium carbonate (1.62 g). The mixture is stirred for 1 h at 100° C. and then poured into ice-cold water. The resulting precipitate is filtered off, washed with water and dried under reduced pressure to give tert-butyl 4-[1-(cyanomethyl)-2,4-dioxo-6-phenyl-1,4-dihydrothieno[3,2-d]pyrimidin-3(2H)-yl]piperidine-1-carboxylate (compound B14a) as a solid, which is used without further purification for the next step.

1. additionpoured into ice-cold water
2. filtrationThe resulting precipitate is filtered off
3. washwashed with water
4. customdried under reduced pressure