HRID1439535

反应详情

EQUATION

反应方程式

HRID 1439535 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

86.8 g (0.1 mol) of 1,1-bis-(4-hydroxyphenyl)-cyclo hexane are suspended in 500 ml of water and 300 ml of methylene chloride at about 0° to 3° C. 20 ml (0.4 mol) of cyanogen chloride are added to this suspension and a solution of 10.6 g (0.1 mol) of Na2CO3 in 50 ml of water is added dropwise over the course of 90 minutes at the same temperature, with vigorous stirring, in such a way that a pH value between 7.5 and 8.5 is maintained in the reaction mixture. Thereafter, 1 N NaOH is added at 0° C in such a way that the abovementioned pH value is maintained, and persists as the final value. Thereafter, the organic phase is separated off and washed with 50 ml of water and the solvent is stripped off at room temperature. 29 g (99% of theory) of 1-(4-hydroxyphenyl)-1-(4-cyanatophenyl)-cyclohexane are thus obtained.

WORKUP

后处理

  1. customat about 0° to 3° C
  2. temperaturein such a way that a pH value between 7.5 and 8.5 is maintained in the reaction mixture
  3. temperatureis maintained
  4. customThereafter, the organic phase is separated off
  5. washwashed with 50 ml of water
  6. customis stripped off at room temperature