反应详情

温度

70 °C

In a 250 ml RBF 2-chloro-5-(ethoxymethyl)pyrimidine (280 mg, 1.622 mmol) and 2-[(1S,2R)-2-(piperidin-4-yl)cyclopropyl]ethanol (334 mg, 1.622 mmol) were dissolved in DMF (1622 μl). Cesium carbonate (1586 mg, 4.87 mmol) was added and the mixture stirred at 70° C. overnight. The mixture was diluted with 4:1 water:brine (200 ml), extracted with EtOAc (3×100 ml), the organic fractions combined, washed with brine, dried over Na2SO4, filtered and the volatiles removed in vacuo. The mixture was purified on a 100 g Biotage HP-SiO2 cartridge using a gradient eluant of 0-100% EtOAc:hexanes to afford the title compound. LC/MS (m/z): 306 (M+H)+.

1. extractionbrine (200 ml), extracted with EtOAc (3×100 ml)
2. washwashed with brine
3. dry with materialdried over Na2SO4
4. filtrationfiltered
5. customthe volatiles removed in vacuo
6. customThe mixture was purified on a 100 g Biotage HP-SiO2 cartridge