HRID1049671

反应详情

EQUATION

反应方程式

HRID 1049671 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

19 g (53 mmol) of methyltriphenylphosphonium bromide [1779-49-3] are suspended in dried THF under protective gas, and 6 g (53 mmol) of potassium tert-butoxide are added in portions at 0° C.; an immediate colour change to orange occurs. 14 g (51.2 mmol) of N,N-diphenyl-p-aminobenzaldehyde [4181-05-9] are added to the reaction solution at 0° C. The mixture is warmed to room temperature and stirred for a further 20 h. The solvent is stripped off in vacuo, the residue is taken up in dichloromethane, the solution is extracted with water, dried over magnesium sulfate, filtered, and the solvent is stripped off in vacuo. The yellow oil obtained is chromatographed over silica gel, giving 12 g (44 mmol) (86%) of a white solid having a purity of 99.5%.

WORKUP

后处理

  1. additionare added in portions at 0° C.
  2. extractionthe solution is extracted with water
  3. dry with materialdried over magnesium sulfate
  4. filtrationfiltered
  5. customThe yellow oil obtained
  6. customis chromatographed over silica gel