HRID1525621

反应详情

EQUATION

反应方程式

HRID 1525621 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
88 °C

PROCEDURE

实验过程

A mixture of ethylene carbonate (14.26 g), xylenes (1.19 g) and 4-hydroxybenzophenone (30.41 g) was heated to 88° C. Sodium iodide (1615 mg) was added. Heating was continued until the temperature of the mixture reached 169° C. The melt was cooled to 110° C. and methanol (12.76 g), sodium hydroxide (50% aqueous solution; 4.01 g), toluene (42.51 g) and water (28.88 g) were added. The lower layer was separated (‘cut’) and discarded. Toluene (18.1 g) was added and the solvents were evaporated by heating to the boiling point of 111° C. 4-(2-Hydroxyethoxy)benzophenone was isolated by crystallisation and filtration at 17° C. resulted in 34.1 g (92%) of beige crystals.

WORKUP

后处理

  1. temperatureHeating
  2. customreached 169° C
  3. temperatureThe melt was cooled to 110° C.
  4. customThe lower layer was separated (‘cut’) and
  5. additionToluene (18.1 g) was added
  6. customthe solvents were evaporated
  7. temperatureby heating to the boiling point of 111° C