反应详情

温度

100 °C

To the compound of Example 12 (4.0 g, 20 mmole) was added POCl3 (15 mL) and the mixture heated at 100° C. for 48 hours. Upon cooling to room temperature the mixture was poured onto crushed ice and then the aqueous phase was extracted with ethyl acetate (2×100 mL). The combined organic extracts were then washed with saturated aqueous sodium bicarbonate (2×50 mL), brine and then dried over MgSO4, filtered and the solvent was evaporated under vacuum to provide 3.46 g of the title compound as a light yellow oil. Thin layer chromatography analysis of the title compound showed a single spot with Rf =0.53 (silica, 4:1 hexanes/ethyl acetate).

1. temperatureUpon cooling to room temperature the mixture
2. additionwas poured
3. customonto crushed ice
4. extractionthe aqueous phase was extracted with ethyl acetate (2×100 mL)
5. washThe combined organic extracts were then washed with saturated aqueous sodium bicarbonate (2×50 mL), brine
6. dry with materialdried over MgSO4
7. filtrationfiltered
8. customthe solvent was evaporated under vacuum