反应详情

19.2 g of 2-tert-butyl-4-piperazin-1-yl-6-cyclopropyl-pyrimidine (73.7 mmol) were dissolved in 50 ml of toluene. 14.6 ml of 1-bromo-3-chloropropane (147.4 mmol) and 3.4 g of sodium hydroxide (84.7 mmol) were added, followed by dropwise addition of 0.95 g of tetrabutylammonium bromide (2.95 mmol, dissolved in water). After stirring for 5 h at 60° C. additional 1-bromo-3-chloropropane was added to drive the reaction to completion. The reaction mixture was cooled, water was added and the product extracted 3 times with ethyl acetate. The organic layers were dried over magnesium sulfate, filtered, and the solvent was evaporated. The crude product was purified by chromatography on silica gel using dichloromethane/ethyl acetate (9:1). Fractions containing the product were combined, the solvent was evaporated to yield 15.4 g of the title compound.

1. additionwas added
2. customthe reaction to completion
3. temperatureThe reaction mixture was cooled
4. extractionthe product extracted 3 times with ethyl acetate
5. dry with materialThe organic layers were dried over magnesium sulfate
6. filtrationfiltered
7. customthe solvent was evaporated
8. customThe crude product was purified by chromatography on silica gel
9. additionFractions containing the product
10. customthe solvent was evaporated