反应详情

Compound 2C (1.65 g, 5.6 mmol) dissolved in DMF (15 ml) was added with K2CO3 (1.1 equiv., 854 mg) and ethyl iodide (1.1 equiv., 0.63 ml) and the reaction was stirred at rt overnight. The reaction was diluted with ethyl acetate and washed several times with water and finally with Brine. The organic phase was dried over sodium sulfate and concentrated under vacuum. The purification of the crude residue by crystallization from ethyl ether and petroleum ether afforded 1.6 g of a semisolid. Yield=88%. 1HNMR (DMSO, 200 MHz) δ 1.00 (3H, d, J=6.2 Hz), 3.32 (3H, s), 3.34 (2H, m), 3.75 (2H, m), 4.42 (1H, t), 5.08 (1H, bs), 7.62 (2H, m), 7.76 (2H, m)

1. washwashed several times with water
2. dry with materialThe organic phase was dried over sodium sulfate
3. concentrationconcentrated under vacuum
4. customThe purification of the crude residue
5. customby crystallization from ethyl ether and petroleum ether