HRID377115

反应详情

EQUATION

反应方程式

HRID 377115 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a solution of sodium hydroxide (5 g) in water (30 ml), were added methylene chloride (100 ml), 5-ethyl-2-pyridineethanol (15 g) and benzyltributylammonium chloride (50% aqueous solution, 6 g), p-toluenesulfonyl chloride (23 g), and the mixture was stirred at room temperature for 2 hours. To the reaction mixture were added p-hydroxybenzaldehyde (12 g), water (100 ml) and sodium hydroxide (8 g) and the mixture was stirred at 40°-50° C. for 12 hours. The reaction mixture was separated into two phases and the methylene chloride layer was dried (MgSO4) and concentrated to give 28.6 g of crude 4-[2-(5-ethyl-2-pyridyl)ethoxy]benzaldehyde as oil. This oil was purified by silica gel chromatography to give 15.8 g (62%) of pure 4-[2-(5-ethyl-2-pyridyl)ethoxy]benzaldehyde as oil.

WORKUP

后处理

  1. stirringthe mixture was stirred at 40°-50° C. for 12 hours
  2. customThe reaction mixture was separated into two phases
  3. dry with materialthe methylene chloride layer was dried (MgSO4)
  4. concentrationconcentrated