HRID465399

反应详情

EQUATION

反应方程式

HRID 465399 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
190 °C

PROCEDURE

实验过程

Into a mixture of 9.50 g (30.9 mmol) of methyl 4-tridecylpyrrole-2-carboxylate obtained in Synthesis Example 3,200 ml of ethylene glycol and 10 ml of water, was added 20 g of potassium hydroxide and the mixture was heated at 190° C. under stirring for 5 hours. After cooling, the mixture was added with water and extracted with ethyl acetate. The organic layer was collected, washed with water, dried over anhydrous magnesium sulfate and then evaporated. The residue was purified by a silica-gel column chromatography (eluent: ethyl acetate/hexane=1/5) to obtain 7.50 g of 3-tridecylpyrrole. The yield was 97% and the melting point was 32.5° to 33.5° C.

WORKUP

后处理

  1. temperatureAfter cooling
  2. extractionextracted with ethyl acetate
  3. customThe organic layer was collected
  4. washwashed with water
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customevaporated
  7. customThe residue was purified by a silica-gel column chromatography (eluent: ethyl acetate/hexane=1/5)