反应详情

A suspension of Intermediate 19 (0.15 g, 0.789 mmol) in phosphorous oxychloride (ALDRICH, 1 ml, 10.73 mmol) was heated under reflux for 1 h. The reaction mixture was added dropwise into iced water, neutralized with solid Na2CO3 and product was extracted with DCM. The combined organic layers were washed with brine and dried over anhydrous Na2SO4. The crude mixture was purified by flash chromatography (Si, eluting with Hexane:EtOAc mixtures from 100:0 to 40:60%) to yield the title compound as a white solid.

1. temperaturewas heated
2. temperatureunder reflux for 1 h
3. extractionwas extracted with DCM
4. washThe combined organic layers were washed with brine
5. dry with materialdried over anhydrous Na2SO4
6. customThe crude mixture was purified by flash chromatography (Si, eluting with Hexane:EtOAc mixtures from 100:0 to 40:60%)