反应详情

温度

80 °C

A mixture of compound 1C (3.0 g, 8.15 mmol), compound 1F (2.85 g, 8.15 mmol), tetrakistriphenylphosphine palladium (471 mg, 0.408 mmol), and sodium carbonate (3.09 g, 29.2 mmol) in tetrahydrofuran (THF)/water (50 mL/30 mL) was degassed for about 45 minutes. The mixture then heated to reflux (about 80° C.) overnight under argon. After cooling to RT, the reaction mixture was poured into DCM (300 mL) then washed with saturated sodium bicarbonate (200 mL), water (200 mL), and brine (200 mL). The organic phase was then collected, dried over magnesium sulfate, and loaded onto silica gel. A flash column (gradient of 25% to 40% ethyl acetate in DCM) and precipitation from ethyl acetate/methanol gave 2.34 g of HTH-1; 56% yield, pure by HNMR.

1. customwas degassed for about 45 minutes
2. temperatureThe mixture then heated
3. temperatureAfter cooling to RT
4. additionthe reaction mixture was poured into DCM (300 mL)
5. washthen washed with saturated sodium bicarbonate (200 mL), water (200 mL), and brine (200 mL)
6. customThe organic phase was then collected
7. dry with materialdried over magnesium sulfate
8. customA flash column (gradient of 25% to 40% ethyl acetate in DCM) and precipitation from ethyl acetate/methanol
9. customgave 2.34 g of HTH-1