反应详情

温度

90 °C

A mixture of 7b (0.14 g, 2.1 eq), 6a (0.1 g, 0.3 mmol) and potassium carbonate (0.1 g, 2.2 eq) in 1 mL of DMA was heated up to 90° C. for 48 h then cooled down to room temperature and diluted with DCM (2 mL) and brine (2 mL). The layers were separated and the aqueous extracted with DCM (2×2 mL). The combined extracts were washed with brine (2×50 mL), dried over magnesium sulfate, filtered and evaporated. The residue was diluted with acetonitrile and purified on preparative HPLC to afford 7c.

1. temperaturethen cooled down to room temperature
2. customThe layers were separated
3. extractionthe aqueous extracted with DCM (2×2 mL)
4. washThe combined extracts were washed with brine (2×50 mL)
5. dry with materialdried over magnesium sulfate
6. filtrationfiltered
7. customevaporated
8. additionThe residue was diluted with acetonitrile
9. custompurified on preparative HPLC