HRID724425
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
CONDITIONS
反应条件
- 温度
- 150 °C
PROCEDURE
实验过程
2,6-Dichlorobenzyl bromide (1.20 g, 5 mmol) was mixed with triethyl phosphite (1.66 g, 10 mmol) and heated at 150° C. for 2 h. The resulting mixture was then distilled at 160° C. under reduced pressure (10 mm Hg) to remove the excess triethyl phosphite. (2,6-Dichloro-benzyl)-phosphonic acid diethyl ester was obtained as a colorless liquid (1.46 g, 100%). 1H NMR (300 MHz, CDCl3) δ 7.33–7.28 (m, 2H), 7.15–7.07 (m, 1H), 4.14–4.02 (m, 4H), 3.60 (d, 2H, J=22.4 Hz), 1.27 (t, 6H, J=7.0 Hz).
WORKUP
后处理
- distillationThe resulting mixture was then distilled at 160° C. under reduced pressure (10 mm Hg)
- customto remove the excess triethyl phosphite