反应详情

温度

90 °C

Compound 9 (3.5 g, 7.96 mmol) and phosphorus oxychloride (20 mL) were combined under argon then heated at 90° C. for 0.5 h. The solution was cooled and poured onto ice. The resulting suspension was made basic with 2N sodium hydroxide and extracted several times with methylene chloride. The combined organic extracts were washed with brine and dried with anhydrous sodium sulfate. Evaporation of the solvent in vacuo gave an oil which was purified by flash column chromatography (hexane ethyl acetate 80:20) to give Compound 10 as a foam: 2.9 g (6.4 mmol, 80%)

1. temperatureThe solution was cooled
2. additionpoured onto ice
3. extractionextracted several times with methylene chloride
4. washThe combined organic extracts were washed with brine
5. dry with materialdried with anhydrous sodium sulfate
6. customEvaporation of the solvent in vacuo
7. customgave an oil which
8. customwas purified by flash column chromatography (hexane ethyl acetate 80:20)