反应详情

0.31 g of sodium hydride (7.8 mmol; 60% in paraffin) was washed oil-free with pentane before 1.3 g of 3-[4-(2-tert-butyl-6-cyclobutyl-pyrimidin-4-yl)-piperazin-1-yl]-propan-1-ol (3.91 mmol) dissolved in 20 ml of dioxane were added. The reaction was heated to reflux for 1 h. After cooling, 0.7 g of 2-chloro-pyrimidine (6.11 mmol) dissolved in 10 ml of dioxane were added. The reaction mixture was heated under reflux for 2 h. The reaction mixture was partitioned between water and ethyl acetate. The organic layer was dried over magnesium sulfate, filtered, the solvent evaporated, and the residue re-dissolved in isopropanol and treated with hydrochloric acid in diethyl ether. After removing most of the organic phase, the residue was treated with isopranol/diisopropyl ether, which, after cautious evaporation, yielded 1.6 g of the title compound.

1. additionwere added
2. temperatureThe reaction was heated
3. temperatureto reflux for 1 h
4. temperatureAfter cooling
5. additionwere added
6. temperatureThe reaction mixture was heated
7. temperatureunder reflux for 2 h
8. customThe reaction mixture was partitioned between water and ethyl acetate
9. dry with materialThe organic layer was dried over magnesium sulfate
10. filtrationfiltered
11. customthe solvent evaporated
12. dissolutionthe residue re-dissolved in isopropanol
13. additiontreated with hydrochloric acid in diethyl ether
14. customAfter removing most of the organic phase
15. additionthe residue was treated with isopranol/diisopropyl ether, which
16. customafter cautious evaporation