反应详情

A suspension of Intermediate 17 (0.225 g, 1.171 mmol) in phosphorous oxychloride (ALDRICH, 0.327 ml, 3.51 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. A brown oil was obtained upon solvent removal in vacuo which 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. customA brown oil was obtained upon solvent removal in vacuo which
7. customwas purified by flash chromatography (Si, eluting with Hexane:EtOAc mixtures from 100:0 to 40:60%)