反应详情

温度

130 °C

A mixture of compound D9 (1 g, 4.148 mmol) and phosphorus(V) oxychloride (2 ml) was subjected to microwave heating at 130° C. for 15 min. After cooling to room temperature, the solvent was evaporated in vacuo. The residue thus obtained was then treated with NaHCO3 (aqueous sat. solution) and extracted with DCM. The organic layer was separated, dried (MgSO4) and evaporated in vacuo. The crude product was purified by column chromatography (silica gel; Et2O as eluent). The desired fractions were collected and evaporated in vacuo to yield compound D10 (0.6 g, 56%) as yellow solid.

1. temperatureAfter cooling to room temperature
2. customthe solvent was evaporated in vacuo
3. customThe residue thus obtained
4. extractionextracted with DCM
5. customThe organic layer was separated
6. dry with materialdried (MgSO4)
7. customevaporated in vacuo
8. customThe crude product was purified by column chromatography (silica gel; Et2O as eluent)
9. customThe desired fractions were collected
10. customevaporated in vacuo
11. customto yield compound D10 (0.6 g, 56%) as yellow solid