反应详情

[4-Amino-2-(piperidin-4-ylamino)-pyrimidin-5-yl]-(2,3-difluoro-6-methoxy-phenyl)-methanone (308 mg, 0.848 mmol, Example 107) in dioxane (3 mL) and sulfamide (814 mg, 8.48 mmol, Aldrich) refluxed overnight. The mixture was diluted with water and sodium bicarbonate and extracted with dichloromethane. The organic solution was washed with water, dried (MgSO4), filtered and evaporated. Chromatography on silica gel (methanol/triethylamine/ethyl acetate 5:2:95) gave, after crystallization from ethanol/ethyl ether, 255 mg of colorless solid, MP 217–218° C. MS(ES) MH+ 443

1. extractionextracted with dichloromethane
2. washThe organic solution was washed with water
3. dry with materialdried (MgSO4)
4. filtrationfiltered
5. customevaporated
6. customChromatography on silica gel (methanol/triethylamine/ethyl acetate 5:2:95) gave
7. customafter crystallization from ethanol/ethyl ether, 255 mg of colorless solid, MP 217–218° C