HRID5549

反应详情

EQUATION

反应方程式

HRID 5549 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
55 °C

PROCEDURE

实验过程

Following the general methods outlined by Weller and Luellen (see above), to a solution of 16.6 g (0.1 mole) of 2,4-dimethoxybenzaldehyde 1 and 20 ml (0.2 mole) of 2-acetylfuran 2 in 100 ml of methanol was added 5.5 g of potassium hydroxide previously dissolved in a small amount of methanol. The resulting mixture was heated to reflux and then stirred overnight at 55° C. The solution was then poured into water acidified with 1N HCl and extracted with CH2Cl2. The CH2Cl2 extracts were dried (Na2SO4) and the solvents removed at high vacuum. The resulting amber oil solidified on standing overnight affording 36.7 g of crude dione 3.

WORKUP

后处理

  1. temperatureThe resulting mixture was heated
  2. temperatureto reflux
  3. extractionextracted with CH2Cl2
  4. dry with materialThe CH2Cl2 extracts were dried (Na2SO4)
  5. customthe solvents removed at high vacuum
  6. waiton standing overnight
  7. customaffording 36.7 g of crude dione 3