HRID1534094

反应详情

EQUATION

反应方程式

HRID 1534094 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-70 °C

PROCEDURE

实验过程

73.7 g (0.655 mol) of potassium tert-butanolate were added a little at a time to 117.6 g (0.269 mol) of bromomethyltriphenylphosphonium bromide in 420 ml of dry tetrahydrofuran at 25° C. while cooling. The reaction mixture was then stirred for half an hour and, at -70° C., a solution of 50 g (0.218 mol) of 3,5-di-tertbutylbenzaldehyde in 120 ml of dry tetrahydrofuran was added dropwise. After half an hour, the mixture was allowed to warm to room temperature, and was then stirred overnight and poured into water. Extraction with ether, washing of the organic phase with water, drying over sodium sulfate and evaporation of the solvent produced a viscous residue.

WORKUP

后处理

  1. temperaturewhile cooling
  2. waitAfter half an hour
  3. temperatureto warm to room temperature
  4. stirringwas then stirred overnight
  5. extractionExtraction with ether
  6. washwashing of the organic phase with water
  7. dry with materialdrying over sodium sulfate and evaporation of the solvent
  8. customproduced a viscous residue