HRID2236333

反应详情

EQUATION

反应方程式

HRID 2236333 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 4-hydroxystyrene (1.22 g, 10 mmol) in ethyl ether 140 mL was added chloroacetic chloride (2.26 g, 20 mmol) and Et3N (1.62 g, 16 mmol). After it was stirred for 2 h, the mixture was washed with brine and water. The ether solution was dried over Na2SO4 and concentrated. After purification by flash column, the 4-chloroacetoxystyrene (1.8 g, 92%) was obtained. Data are: 1H NMR (CDCl3, 300 MHz) δ 7.46 (d, 2H, J=1.8 Hz), 7.11 (d, 2H, J=8.4 Hz), 6.73 (dd, 1H, J=17.7 Hz), 5.74 (d, 1H, J=18 Hz), 5.29 (d, J=1.1 Hz), 4.31 (s, 2H). 13C NMR (CDCl3, 75 MHz) δ 166.0, 150.0, 136.0, 135.8, 127.4, 121.3, 114.6, 41.0.

WORKUP

后处理

  1. washthe mixture was washed with brine and water
  2. dry with materialThe ether solution was dried over Na2SO4
  3. concentrationconcentrated
  4. customAfter purification by flash column