反应详情

温度

85 °C

Intermediate VI (63 g, 0.198 mol) and POCl3 (5 v/w, 315 in L) were added to acetonitrile (5 v/w, 315 mL). The mixture was warmed up to 85° C. to react under reflux for 6 h. After completion of the reaction, the reaction solution was cooled. POCl3 and acetonitrile were evaporated off to produce a grey viscous solid. This solid was added to a great deal of ice-water mixture, adjusted with a 10% KOH solution to a pH of 10, and extracted with CH2Cl2 (200 mL×3). The organic layer was collected, dried over anhydrous sodium sulfate, and cooled after evaporating off the solvate to produce an off-white solid (58 g) in a yield of 87.3%.

1. customto react
2. temperatureunder reflux for 6 h
3. customAfter completion of the reaction
4. temperaturethe reaction solution was cooled
5. customPOCl3 and acetonitrile were evaporated off
6. customto produce a grey viscous solid
7. extractionextracted with CH2Cl2 (200 mL×3)
8. customThe organic layer was collected
9. dry with materialdried over anhydrous sodium sulfate
10. temperaturecooled
11. customafter evaporating off the solvate