HRID888672

反应详情

EQUATION

反应方程式

HRID 888672 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

After magnesium (0.63 g; 25.8 mmol) and anhydrous THF (25 ml) were put into a flask, 2-bromo-3-dodecylthiophene (7.78 g; 23.5 mmol) was slowly added thereto. After starting Grignard reaction, the solution was refluxed until magnesium was almost removed. The purified DMF (3.65 g; ˜4 ml; 50 mmol) was slowly added dropwise to the reaction solution. The reaction solution was refluxed for one day, and cooled to 0° C., and 5% HCl (100 ml) was added thereto to terminate the reaction. An organic layer was extracted by using ethyl ether, and the obtained organic layer was washed sequentially with NaHCO3, a saturated NaCl aqueous solution, and water. The residual moisture was removed over anhydrous magnesium sulfate. After removing the solvent, the residue was subjected to a column separation process by using silica gel (ethyl acetate/hexane=1/9) to obtain 3-dodecylthiophene-2-carboaldehyde (3.6 g; 55%).

WORKUP

后处理

  1. customGrignard reaction
  2. customwas almost removed
  3. temperatureThe reaction solution was refluxed for one day
  4. customto terminate
  5. customthe reaction
  6. extractionAn organic layer was extracted
  7. washthe obtained organic layer was washed sequentially with NaHCO3
  8. customThe residual moisture was removed over anhydrous magnesium sulfate
  9. customAfter removing the solvent
  10. customthe residue was subjected to a column separation process