HRID1252468

反应详情

EQUATION

反应方程式

HRID 1252468 的结构方程式

CONDITIONS

反应条件

温度
10 °C

PROCEDURE

实验过程

Phosphorus oxychloride (26.75 g, 0.174 mol) was added dropwise to dimethylformamide (12.92 g, 0.177 mol). This mixture was cooled to 10° C. for 1/2 hour, then 2-t-butylfuran (18.45 g, 0.149 mol) was added dropwise and the mixture stirred at room temperature for 3 hours. The mixture was poured into ice/water, neutralised with sodium carbonate and extracted into diethyl ether. The ethereal extracts were washed with water, dried over anhydrous sodium sulphate and the solvent removed to give a brown oil. Purification by column chromatography (silica eluted with petroleum ether/ethyl acetate 9:1) gave 5-t-butyl-2-furancarboxaldehyde (22.46 g, 99%).

WORKUP

后处理

  1. extractionextracted into diethyl ether
  2. washThe ethereal extracts were washed with water
  3. dry with materialdried over anhydrous sodium sulphate
  4. customthe solvent removed
  5. customto give a brown oil
  6. customPurification
  7. washby column chromatography (silica eluted with petroleum ether/ethyl acetate 9:1)