反应详情

温度

100 °C

A mixture of N-(4-fluoro-phenyl)-N′-methyl-pyrimidine-4,6-diamine (2.18 g, 10 mmol), 4-methoxyphenyl isocyanate (1.29 mL, 10 mmol) and dibutyltin diacetate (0.54 mL, 2 mmol) in dry dioxane (20 mL) is shaken for 6 h at 100° C. After addition of a second portion of 4-methoxyphenyl isocyanate (0.9 mL, 7 mmol) stirring is continued at 100° C. for 9 h. The reaction mixture is treated with ethyl acetate and half-saturated Na2CO3 solution. The organic layer is filtered, dried over Na2SO4, evaporated, and the residue purified by flash chromatography (hexane/ethyl acetate). The combined pure fractions are evaporated, the residue is suspended in hot CH3OH and the hot mixture filtered. This procedure is repeated several times. The solid thus obtained is dried in vacuo to afford the title compound.

1. stirringstirring
2. waitis continued at 100° C. for 9 h
3. filtrationThe organic layer is filtered
4. dry with materialdried over Na2SO4
5. customevaporated
6. customthe residue purified by flash chromatography (hexane/ethyl acetate)
7. customThe combined pure fractions are evaporated
8. filtrationthe hot mixture filtered
9. customThe solid thus obtained
10. customis dried in vacuo