反应详情

温度

130 °C

A mixture of 8-7 (5.5 g, 10.2 mmol) and POCl3 (50.0 g, 326.1 mmol) and DMF (0.3 g, 4.1 mmol) was heated to reflux at 130° C. for 3 hr. The reaction mixture was cooled and concentrated to remove POCl3. 40 mL Toluene was added and concentrated to obtain a solid. To the solid was added 50 mL H2O and 40 mL NaHCO3 (saturated) and 20 mL 1NNaOH to pH=9. The mixture was stirred to precipitate a solid which was collected via filtration as the desired product 8-8. It was washed by water and CH3CN and dried under vacuum.

1. temperaturewas heated
2. temperatureThe reaction mixture was cooled
3. concentrationconcentrated
4. customto remove POCl3
5. addition40 mL Toluene was added
6. concentrationconcentrated
7. customto obtain a solid
8. customto precipitate a solid which
9. filtrationwas collected via filtration as the desired product 8-8
10. washIt was washed by water and CH3CN
11. customdried under vacuum