HRID278039

反应详情

EQUATION

反应方程式

HRID 278039 的结构方程式

PROCEDURE

实验过程

Under nitrogen atmosphere, 20.9 g of this crude aldehyde was dissolved in 300 ml of dioxane, followed by the addition of 50.9 g of dichlorodicyanobenzo-quinone. The resulting mixture was heated under reflux for 1.5 hours and cooled to room temperature by allowing to stand. Then, 500 ml of toluene was added to the resulting mixture to thereby form a precipitate. The resulting precipitate-containing mixture was filtered and the filter cake was washed with toluene several times. The filtrate was concentrated and the resulting crude product was purified by silica gel column chromatography to give 10.3 g of the title compound as colorless crystals.

WORKUP

后处理

  1. temperatureThe resulting mixture was heated
  2. temperatureunder reflux for 1.5 hours
  3. customto thereby form a precipitate
  4. additionThe resulting precipitate-containing mixture
  5. filtrationwas filtered
  6. washthe filter cake was washed with toluene several times
  7. concentrationThe filtrate was concentrated
  8. customthe resulting crude product was purified by silica gel column chromatography