反应详情

温度

120 °C

A solution of 2e from Example 3 (30 g, 0.15 mol) in dry DMF (200 ml) is cooled to 0° C. under nitrogen. Sodium hydride (7.2 g of a 60% dispersion in mineral oil) is added portionwise. When the evolution of hydrogen has ceased a solution of 1c from Example 1 (52 g, 0.19 mol) in 50 ml DMF is added. The mixture is stirred at 120° C. for 5 hours and left at ambient temperature over night. The reaction mixture is poured into four volumes of water and the crude product is filtered off. Purification on silica gel using a mixture of ethyl acetate and petroleum ether (3:17) as the eluent affords pure 6c as an oil (17 g, 25%).

1. additionis added
2. waitleft at ambient temperature over night
3. filtrationthe crude product is filtered off
4. customPurification on silica gel using
5. additiona mixture of ethyl acetate and petroleum ether (3:17) as the eluent