反应详情

A solution of benzyl 4-bromo-but-2-enate (430 mg, 1.68 mmol) and triphenylphosphine (661 mg, 2.52 mmol) in benzene (3 ml) was stirred at room temperature under nitrogen for 20 hours. The resulting white solid was collected through filtration and washed with benzene (3×2 ml), and dried at 100° C. under vacuum to give the title compound (510 mg, 59% yield). 1H NMR (CD3OD): δppm 4.60 (2H, m, slowly disappeared due to deuterium exchange), 5.13 (2H, s), 6.16 (1H, dd, J1=15.3 Hz, J2=1.1 Hz), 6.81 (1H, m), 7.33 (5H, m), 7.78 (12 H, m), 7.90 (3H, m). 13C NMR (CD3OD): δppm 67.6 (t), 68.1 (t), 118.3 (s), 118.8 (s), 119.4 (s), 120.0 (s), 129.3 (d), 129.4 (d), 129.5 (d), 129.6 (d), 129.7 (d), 131.4 (d), 131.5 (d), 131.7 (d), 134.7 (d), 134.85 (d), 134.94 (d), 135.1 (d), 135.2 (d), 135.3 (d), 136.5 (d), 136.6 (d), 136.69 (d), 136.73 (d), 155.7 (s); 165.8 (s).

1. filtrationThe resulting white solid was collected through filtration
2. washwashed with benzene (3×2 ml)
3. customdried at 100° C. under vacuum