反应详情

温度

40 °C

Isopropyl 4-bromobutyrate (16.0 g, 76.5 mmol) and triphenylphosphine (20.0 g, 76.5 mmol) in toluene (160 ml) were heated at reflux under nitrogen for 39 h. The mixture was allowed to cool (to approx 40° C.), filtered and the solid was washed with toluene (3 ×25 ml). The product was dried under vacuum to give a white solid (20.7 g, 57%); m.p. 198° C. (onset by DSC); 1H NMR (200 MHz, CDCl3) δ ppm 7.85-7.60 (15 H, m), 4.89 (1 H, heptet, J 6), 3.96-3.70 (2 H, m), 2.75 (2 H, t, J 6), 1.95-1.75 (2 H, m) and 1.13 (6 H, d, J 6).

1. temperatureat reflux under nitrogen for 39 h
2. filtrationfiltered
3. washthe solid was washed with toluene (3 ×25 ml)
4. customThe product was dried under vacuum