反应详情

温度

90 °C

The product from step (ii) (6.6 g) was added to phosphorous oxychloride (40 ml) under nitrogen. The resulting mixture was stirred at 90° C. for 15 h. The phosphorous oxychloride was evaporated under reduced pressure and the residue cautiously diluted with water (50 mL). The aqueous phase was neutralised with NaHCO3 and heated at 50° C. for 1 h. The mixture was allowed to cool and the precipitate was collected by filtration. The solid was suspended in MeCN (40 mL) and collected by filtration to give the subtitle compound as a cream solid 3.70 g that was used without further purification.

1. customThe phosphorous oxychloride was evaporated under reduced pressure
2. additionthe residue cautiously diluted with water (50 mL)
3. temperatureheated at 50° C. for 1 h
4. temperatureto cool
5. filtrationthe precipitate was collected by filtration
6. filtrationcollected by filtration