反应详情

14.8 g 2-tert-butyl-4-hydroxy-6-cyclopropyl-pyrimidine (76.9 mmol) were dissolved in 100 ml of toluene and 3 ml of dimethylformamide. 23.6 ml of POCl3 (153.7 mmol) were added dropwise at 10° C. After stirring overnight at room temperature most of the toluene was evaporated. The mixture was cooled with ice and 20 ml of water were added cautiously. Subsequently, an additional 200 ml of water were added and the aqueous phase was extracted four times with dichloromethane. The combined organic phases were dried over magnesium sulfate, filtered, and then concentrated to dryness to yield 17 g of a yellowish oil (quant.).

1. customwas evaporated
2. temperatureThe mixture was cooled with ice and 20 ml of water
3. additionwere added cautiously
4. additionSubsequently, an additional 200 ml of water were added
5. extractionthe aqueous phase was extracted four times with dichloromethane
6. dry with materialThe combined organic phases were dried over magnesium sulfate
7. filtrationfiltered
8. concentrationconcentrated to dryness