反应详情

温度

110 °C

A mixture of methyl 2-(2-chloro-4-methyl-6-phenylpyrimidin-5-yl)acetate (200 mg; 0.723 mmol) and piperidine (0.286 mL; 2.89 mmol) in THF (2 mL) was placed in a sealed tube and heated via microwave irradiation at 110° C. for 1 h. The reaction mixture was diluted with a saturated sodium hydrogen carbonate solution and extracted twice with ethyl acetate. The organic layers were combined, washed with brine, dried over magnesium sulphate and concentrated under vacuum. The crude material was purified by flash chromatography on silica gel using a linear gradient of ethylacetate (2-20%) in heptane to give 158 mg (63%) of methyl 2-(4-methyl-6-phenyl-2-(piperidin-1-yl)pyrimidin-5-yl)acetate. ESI/APCI(+): 326 (M+H).

1. customwas placed in a sealed tube
2. extractionextracted twice with ethyl acetate
3. washwashed with brine
4. dry with materialdried over magnesium sulphate
5. concentrationconcentrated under vacuum
6. customThe crude material was purified by flash chromatography on silica gel using a linear gradient of ethylacetate (2-20%) in heptane