反应详情

A mixture of the product from Step 79b (1.28 g, 4.70 mmol, 1 eq), benzene (8 mL), and POCl3 (2.0 mL, 21 mmol) is heated under reflux for 65 h and cooled. The mixture is then evaporated and extracted between CHCl3 and water. The organic layer is separated, dried over MgSO4, filtered, and evaporated. The residue is crystallized from EtOH to give the title product (0.61 g, 51%). MS (ESI) for C12H10ClNO3 m/z 252 (M+H)+.

1. temperatureis heated
2. temperatureunder reflux for 65 h
3. temperaturecooled
4. customThe mixture is then evaporated
5. extractionextracted between CHCl3 and water
6. customThe organic layer is separated
7. dry with materialdried over MgSO4
8. filtrationfiltered
9. customevaporated
10. customThe residue is crystallized from EtOH