HRID1439533

反应详情

EQUATION

反应方程式

HRID 1439533 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

28.4 g (0.1 mol) of 2,2-bis-(3,5-dimethyl-4-hydroxyphenyl)-propane are suspended in 500 ml of water and 300 ml of dichloromethine. After cooling to 0° C, 15 ml (0.3 mol) of cyanogen chloride are added. 10.6 g (0.1 mol) of Na2CO3, dissolved in 50 ml of water, are then added dropwise over the course of 2 hours, with vigorous stirring, in such a way that a pH value of between 7.5 and 8.5 is maintained constantly in the reaction mixture. At the same time, the reaction temperature is kept at about 0° C by cooling. Thereafter, the reaction is terminated by slow addition of 1 N NaOH, the 1 N NaOH being added in such a way that a pH value of 7.5 to 8.0 is constantly maintained in the reaction mixture and persists as the final value. After the end of the reaction, the organic phase is separated off, washed with 50 ml of water and concentrated at room temperature. 30.8 g (99% of theory) of 2-(3,5-dimethyl-4-hydroxyphenyl)-2-(3,5-dimethyl-4-cyanatophenyl)-propane are obtained as the residue.

WORKUP

后处理

  1. additionare then added dropwise over the course of 2 hours, with vigorous stirring
  2. temperaturein such a way that a pH value of between 7.5 and 8.5 is maintained constantly in the reaction mixture
  3. customis kept at about 0° C
  4. temperatureby cooling
  5. customThereafter, the reaction is terminated by slow addition of 1 N NaOH
  6. additionthe 1 N NaOH being added in such a way that a pH value of 7.5 to 8.0
  7. temperatureis constantly maintained in the reaction mixture and persists as the final value
  8. customAfter the end of the reaction
  9. customthe organic phase is separated off
  10. washwashed with 50 ml of water
  11. concentrationconcentrated at room temperature