反应详情

温度

100 °C

To a homogeneous mixture of phosphorus pentoxide and 85% phosphorus acid at 100° C., was added 5-(3-methoxyphenyl)pentanoic acid in small portions over 20 minutes. The vigorously stirred mixture was heated at 100° C. for 6 hours. Then it was poured on ice-water, and extracted with ether (3 times). The organic phase was washed with water and dried over anhydrous sodium sulfate. Evaporation of the combined organic phase afforded a light yellow oil in more than 95% yield; 1H NMR δ 7.77 (d, 1H, J=8.6 Hz), 6.80 (dd, 1H, J=2.5, 8.6 Hz), 6.69 (d, 1H, J=2.5 Hz), 3.84 (s, 3H), 2.90 (t, 2H, J=6.2 Hz), 2.71 (t, 2H, J=5.9 Hz), 1.91-1.76 (m, 4H).

1. additionThen it was poured on ice-water
2. extractionextracted with ether (3 times)
3. washThe organic phase was washed with water
4. dry with materialdried over anhydrous sodium sulfate
5. customEvaporation of the combined organic phase
6. customafforded a light yellow oil in more than 95% yield