HRID1110487

反应详情

EQUATION

反应方程式

HRID 1110487 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
85 °C

PROCEDURE

实验过程

The compound was prepared according to the procedure described in Example 84. The following reagents were used: 2,2'-difluorobenzophenone (6.0 g) diisopropylamine (28.8 mL) 1.6M n-butyl lithium in hexane (129 mL), acetaldehyde N-tert-butylimine (13.2 mL). diethyl chlorophosphonate (14.85 mL) and tetrahydrofurane (100 mL). The reaction was worked up in the usual manner, with the exception that the oxalic acid catalyzed hydrolysis was slow and it was necessary to heat the mixture to 85° C. for one hour to complete the conversion. The crude product (5.8 g), obtained as an orange oil, was crystallized from hexane to give 4.6 g of 3,3-bis(2-fluorophenyl)-2-propenal mp 75°-77.° C. Anal. Calculated for : C15H10F2O: C. 73.76; H, 4.13; F, 15.56 Found: C, 73.32; H, 4.27; F, 15.74.

WORKUP

后处理

  1. customThe compound was prepared
  2. customhydrolysis
  3. customThe crude product (5.8 g), obtained as an orange oil
  4. customwas crystallized from hexane