HRID375996

反应详情

EQUATION

反应方程式

HRID 375996 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 54.6 g (0.2 mol) of 4-diphenylaminobenzaldehyde, 51.6 g (0.2 mol) of diethyl-4-methoxybenzyl phosphonate, and 250 ml of dimethylformamide was placed in a 500 ml four-neck flask. 57.9 g of 28% sodium methylate was added dropwise to the above mixture with stirring at room temperature over a period of 15 minutes. Thus, the reaction was carried out at 50° to 60° C. for five hours. The thus obtained reaction mixture was diluted with 500 ml of water, and then made acid with the addition of acetic acid. Then the mixture was filtrated to obtain a wet cake. The thus obtained wet cake was washed with 100 ml of methanol three times, and recrystallized from a mixed solvent of ethanol and dioxane, whereby 46.2 g of 4-diphenylamino-4'-methoxystilbene was obtained as yellow crystals in the form of needles in a yield of 61.3%. The melting point of the obtained compound was 170° to 171.5° C.

WORKUP

后处理

  1. customwas placed in a 500 ml four-neck flask
  2. waitThus, the reaction was carried out at 50° to 60° C. for five hours
  3. customThe thus obtained reaction mixture
  4. filtrationThen the mixture was filtrated
  5. customto obtain a wet cake
  6. washThe thus obtained wet cake was washed with 100 ml of methanol three times
  7. customrecrystallized from a mixed solvent of ethanol and dioxane