反应详情

A mixture of the product from step (iii) (2.3 g) and POCl3 (25 ml) was heated under reflux for 8 h. The mixture was evaporated under reduced pressure and ice/water added to the residue. The mixture was stirred at rt for 15 min then neutralised with aq. 2M NaOH solution and heated at 40° C. for 2 h then extracted with DCM. The organics were dried, evaporated under reduced pressure and the residue purified by column chromatography (2% MeOH/DCM), to give the subtitle compound as a solid, 530 mg.

1. temperaturewas heated
2. temperatureunder reflux for 8 h
3. customThe mixture was evaporated under reduced pressure and ice/water
4. additionadded to the residue
5. temperatureheated at 40° C. for 2 h
6. extractionthen extracted with DCM
7. customThe organics were dried
8. customevaporated under reduced pressure
9. customthe residue purified by column chromatography (2% MeOH/DCM)