反应详情

温度

110 °C

A mixture of methyl 2-(2-chloro-4-methyl-6-phenylpyrimidin-5-yl)acetate (200 mg; 0.688 mmol) and piperidine (0.272 mL; 2.75 mmol) in THF (2 mL) was placed in a sealed tube and heated under 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 reduced pressure. The crude material was purified by flash chromatography on silica gel using a linear gradient of ethylacetate (2-20%) in heptane to give 186 mg (87%) of methyl 2-(4-methyl-2-(piperidin-1-yl)-6-p-tolylpyrimidin-5-yl)acetate. ESI/APCI(+): 340 (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 reduced pressure
6. customThe crude material was purified by flash chromatography on silica gel using a linear gradient of ethylacetate (2-20%) in heptane