反应详情

To a stirred solution, cooled to −10° C., of 4.3 g (12.1 mmol) of 5-(2-chlorophenyl) aminomethyl-4-amino-2-benzylthiopyrimidine in 100 mL of tetrahydrofuran was added 3.1 mL (22.2 mmol) of triethylamine. This solution was then treated dropwise with a solution of 6.15 mL of phosgene (20% solution in toluene; 11.8 mmol) After stirring for 30 minutes, an additional 1.0 mL of triethylamine (7.1 mmol) was added followed by 2.0 mL of phosgene (20% solution in toluene; 3.8 mmol). The reaction was warmed to room temperature, treated with 0.5 mL H2O and stirred for 30 minutes. The reaction was then filtered and the mother liquor was concentrated and stirred with dichloromethane. The product was then collected by vacuum filtration and dried in vacuo to give 3.83 g of 7-benzylthio-3-(2-chlorophenyl)-3,4-dihydropyrimido[4,5-d]-pyrimidin-2(1H)-one as a white solid.

1. stirringstirred for 30 minutes
2. filtrationThe reaction was then filtered
3. concentrationthe mother liquor was concentrated
4. stirringstirred with dichloromethane
5. filtrationThe product was then collected by vacuum filtration
6. customdried in vacuo