反应详情

To a stirred solution of (20) (286 mg, 1 mmol), anhydrous powdered potassium carbonate (134 mg, 1 mmol), and lithium iodide (134 mg, 1 mmol) in DMF (5 ml) at room temperature, was added 2-Chloro-4-chloromethyl-pyrimidine (164 mg, 1 mmol). After stirring for overnight, the mixture was evaporated in vacuo and the residue was purified by silica gel column chromatography (eluent, EA:hexanes (1:1)) to afford 210 mg (51%) of a white solid. m.p. 197-198° C.; 1H NMR (300 MHz, CDCl3) δ 1.17 (3H, d, J=6.9 Hz), 1.21 (3H, d, J=6.9 Hz), 2.29-2.39 (7H, m), 4.73 (1H, d, J=17.4 Hz), 4.95 (1H, d, J=17.4 Hz), 7.07 (1H, d, J=5.1 Hz), 7.28 (1H, s), 7.48 (2H, s), 8.46 (1H, d, J=5.1 Hz), 9.41 (1H, s); m/z (EI) 412 (M+).

1. customthe mixture was evaporated in vacuo
2. customthe residue was purified by silica gel column chromatography (eluent, EA:hexanes (1:1))