反应详情

温度

100 °C

To DMF (3.8 mL) at 5° C., was added POCl3 (1.4 mL) dropwise. After 5 minutes, 62b (1 g, 4.9 mmol) was added dropwise in 2 mL of DMF. The mixture was heated to 100° C. overnight. The mixture was allowed to cool to room temperature and was added dropwise to 50 mL of 1N HCl. The solution was extracted 3 times with ethyl acetate. The combined organic layer was dried, evaporated, then purified by column chromatography (eluent: 0 to 30% EtOAc in hexane) to give 0.13 g of 62c (19% yield).

1. temperatureto cool to room temperature
2. extractionThe solution was extracted 3 times with ethyl acetate
3. customThe combined organic layer was dried
4. customevaporated
5. custompurified by column chromatography (eluent: 0 to 30% EtOAc in hexane)