反应详情

Sulfuric acid (1.97 g, 20 mmol) was added dropwise to 5-chloro-2-cyclopropyl-6-(diethoxymethyl)-4-pyrimidinamine (i.e. the product of Example 6) (2.71 g, 10 mmol) in acetonitrile (27.5 mL) at room temperature. The temperature rose to 35° C. When the mixture had cooled to 29° C. ammonium persulfate (0.5 g, 2.21 mmol) was added in one portion. After stirring for 20 h at room temperature the mixture was poured into saturated aqueous sodium bicarbonate solution (100 mL). The mixture was extracted with ethyl acetate (2×70 mL). The combined extracts were dried and evaporated to leave the product as an off-white solid (1.32 g, 55% yield). Product purified by chromatography on silica gel (eluted with 40:60 ethyl acetate-hexanes) followed by washing with hydrochloric acid (1 N) melted at 93-95° C.

1. customrose to 35° C
2. additionwas added in one portion
3. extractionThe mixture was extracted with ethyl acetate (2×70 mL)
4. customThe combined extracts were dried
5. customevaporated