HRID85303

反应详情

EQUATION

反应方程式

HRID 85303 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In a stream of argon, to 300 ml of dioxane were added 21.7 g (100 mmol) of 3,5-dimethoxybromobenzene and 13.0 g (100 mmol) of dibutylamine, and 22.0 g (110 mmol) of potassium bistrimethylsilylamide was added thereto with stirring. After well-stirred, the mixture was heated under reflux with stirring overnight. The reactant was poured into 2 L of ice water and subjected to 3 times of extraction with 200 ml of chloroform. Washing with a saturated saline solution, drying over anhydrous magnesium sulfate, and concentration were performed. The residue was purified by silica gel chromatography to give 23.4 g (yield: 88%) of 4-dibutylamino-3,5-dimethoxybenzene as a colorless transparent oily matter.

WORKUP

后处理

  1. additionwas added
  2. stirringAfter well-stirred
  3. temperaturethe mixture was heated
  4. temperatureunder reflux
  5. stirringwith stirring overnight
  6. extractionsubjected to 3 times of extraction with 200 ml of chloroform
  7. washWashing with a saturated saline solution
  8. dry with materialdrying over anhydrous magnesium sulfate, and concentration
  9. customThe residue was purified by silica gel chromatography