反应详情

A cooled solution of 5-(2-chlorophenyl)aminomethyl-4-phenylamino-2-methylthiopyrimidine (6 g) and 5.2 mL of triethylamine in 75 mL of tetrahydrofuran was added dropwise 8.5 mL of phosgene (20% in toluene) in 35 mL of tetrahydrofuran. The mixture was stirred at room temperature overnight. Additional 3 mL phosgene (20% in toluene) was added to the mixture. After stirring for 15 minutes the mixture was treated with water and ethyl acetate. The phases were separated and the organic phase was washed with brine, dried over sodium sulfate, filtered and evaporated. The crude product was purified by column chromatography using 10:45 ethyl acetate/hexanes as eluant to give 2.1 g of 3-(2-chlorophenyl)-7-methylthio-1-phenyl-3,4-dihydropyrimido[4,5-d]-pyrimidin-2(1H)-one as a white solid, m.p. 79.5-82.4° C.

1. stirringAfter stirring for 15 minutes the mixture
2. customThe phases were separated
3. washthe organic phase was washed with brine
4. dry with materialdried over sodium sulfate
5. filtrationfiltered
6. customevaporated
7. customThe crude product was purified by column chromatography