HRID1380809

反应详情

EQUATION

反应方程式

HRID 1380809 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

Into an ethanol solution (5 liters) comprising 500 g (3.67 moles) of anisaldehyde and 500 g (3.67 moles) of 4-hydroxyacetophenone was dropped an aqueous solution (600 ml) of 250 g of sodium hydroxide in about 80 minutes in a stream of nitrogen. Thereafter, the mixture was heated to 50° C. and agitated for 24 hours. The reaction mixture was cooled down to room temperature, to which were added 2 liters of 12% hydrochloric acid and then 4 liters of water, whereupon crystals settled. The crystals were collected by filtration and quickly washed with ethanol, followed by drying under reduced pressure to obtain 750 g of the intended compound (2.95 moles, yield 80%). The compound was recrystallized from ethanol to obtain light yellow prismatic purified crystals. The melting point and various spectral data of the compound coincided with those of a reference compound.

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled down to room temperature, to which
  2. filtrationThe crystals were collected by filtration
  3. washquickly washed with ethanol
  4. customby drying under reduced pressure