反应详情

3-(2,6-Difluoro-3,5-dimethoxy-phenyl)-1-ethyl-7-methylsulfinyl-3,4-dihydro-1H-pyrimido[4,5-d]pyrimidin-2-one was prepared using 0.50 g (1.21 mmol) of 3-(2,6-difluoro-3,5-dimethoxy-phenyl)-1-ethyl-7-methylsulfinyl-3,4-dihydro-1H-pyrimido[4,5-d]pyrimidin-2-one and 0.59 g (3.64 mmol) of N-(3-amino-propyl)diethanolamine. The crude product was purified using medium-pressure chromatography eluting with a gradient of 9:1 ethyl acetate/methanol to 9:1:0.25 to 9:1:0.5 ethyl acetate/methanol/triethylamine to give 0.43 g (69%) of the title compound: mp 128° C.–129° C. MS (APCI) (m+1)/z 511.2.

1. customThe crude product was purified
2. washeluting with a gradient of 9:1 ethyl acetate/methanol to 9:1:0.25 to 9:1:0.5 ethyl acetate/methanol/triethylamine