反应详情

0.36 g of sodium hydride (9 mmol, 60% in paraffin) were washed oil-free with pentane before 1.5 g of 3-[4-(2-tert-butyl-6-cyclobutyl-pyrimidin-4-yl)-piperazin-1-yl]-propan-1-ol (4.5 mmol) dissolved in 20 ml of dioxane were added. The reaction was heated to reflux for 1 h. After cooling, 0.75 g of 4-chloro-2-methylsulfanyl-pyrimidine (4.67 mmol) dissolved in 10 ml of dioxane were added. The reaction mixture was stirred under reflux for 2 h. The reaction mixture was partitioned between water and ethyl acetate. The organic layer was extracted with 5% aqueous citric acid, the pH of the aqueous phase was adjusted to basic pH with 2 N sodium hydroxide solution. The aqueous layer was re-extracted with ethyl acetate, the organic layer was dried over magnesium sulfate, filtered, and the solvent was evaporated to yield 1.75 g of the title compound as a yellowish oil.

1. additionwere added
2. temperatureThe reaction was heated
3. temperatureto reflux for 1 h
4. temperatureAfter cooling
5. additionwere added
6. temperatureunder reflux for 2 h
7. customThe reaction mixture was partitioned between water and ethyl acetate
8. extractionThe organic layer was extracted with 5% aqueous citric acid
9. extractionThe aqueous layer was re-extracted with ethyl acetate
10. dry with materialthe organic layer was dried over magnesium sulfate
11. filtrationfiltered
12. customthe solvent was evaporated