反应详情

To a solution of methyl 2-(2-chloro-4-methyl-6-p-tolylpyrimidin-5-yl)acetate (3 g; 10.32 mmol) in 2-methyltetrahydrofuran (20 ml) was added piperidine (4.09 mL; 41.3 mmol) and triethylamine (5.72 mL; 41.3 mmol). The reaction was heated under reflux for 5 h and the reaction mixture was partitioned between ethyl acetate and a saturated solution of sodium hydrogen carbonate. The phases were separated and the aqueous layer was extracted twice with ethyl acetate. The combined organic layers were dried over magnesium sulphate, filtered and concentrated under reduced pressure. Purification by flash-chromatography on silica gel using a gradient of ethyl acetate (2-20%) in heptane furnished 1.88 g (48%) of the title compound as a white solid.

1. temperatureThe reaction was heated
2. temperatureunder reflux for 5 h
3. customthe reaction mixture was partitioned between ethyl acetate
4. customThe phases were separated
5. extractionthe aqueous layer was extracted twice with ethyl acetate
6. dry with materialThe combined organic layers were dried over magnesium sulphate
7. filtrationfiltered
8. concentrationconcentrated under reduced pressure
9. customPurification by flash-chromatography on silica gel using a gradient of ethyl acetate (2-20%) in heptane