HRID2255865

反应详情

EQUATION

反应方程式

HRID 2255865 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-20 °C

PROCEDURE

实验过程

A mixture of (2-(1,3-dioxan-2-yl)ethyl)triphenylphosphonium bromide (25.0 g, 54.7 millimols) with THF (150 ml) was cooled down to -20° C., followed by adding t-BuOK (6.1 g, 54.7 millimols) to the mixture, stirring for 30 minutes, dropwise adding to the mixture, a THF (80 ml) solution of trans-4-(trans-4-(4-cyanophenyl)cyclohexyl)cyclohexanecarbaldehyde (14.4 g, 49.8 millimols) so as to keep the temperature at -20° C. or lower, stirring the mixture at the same temperature for 2 hours, and treating the reaction product in the same manner as in Example 2, except that the quantity of ethyl acetate used for extraction was made 400 ml, to obtain raw 4-(trans-4-(trans-4-(3-(1,3-dioxan-2-yl)propenyl)cyclohexyl)cyclohexyl)benzonitrile (17.5 g).

WORKUP

后处理

  1. additiondropwise adding to the mixture
  2. customat -20° C.
  3. stirringlower, stirring the mixture at the same temperature for 2 hours
  4. additiontreating the reaction product in the same manner as in Example 2
  5. extractionexcept that the quantity of ethyl acetate used for extraction