HRID5549
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureThe resulting mixture was heated
- temperatureto reflux
- extractionextracted with CH2Cl2
- dry with materialThe CH2Cl2 extracts were dried (Na2SO4)
- customthe solvents removed at high vacuum
- waiton standing overnight
- customaffording 36.7 g of crude dione 3