HRID2259724

反应详情

EQUATION

反应方程式

HRID 2259724 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 0.028 mole of 3-benzoyl-2-nitrobenzeneacetic acid, 50 mL of thionyl chloride and 50 mL of benzene is heated at reflux. The dark solution is concentrated under vacuum. The residue is diluted with benzene and concentrated under vacuum (twice). A portion of the acid chloride (0.01 3 mole) in tetrahydrofuran is added to a solution of 3-amino (3,4-dimethoxyphenyl)propane (0.015 mole). The mixture is stirred at room temperature and then added to 200 mL of cold water. The resulting mixture is extracted with diethyl ether. The combined extracts are washed with water, dried over sodium sulfate and concentrated under reduced pressure. The residue is purified using standard procedures to give the product.

WORKUP

后处理

  1. temperatureis heated
  2. temperatureat reflux
  3. concentrationThe dark solution is concentrated under vacuum
  4. additionThe residue is diluted with benzene
  5. concentrationconcentrated under vacuum (twice)
  6. extractionThe resulting mixture is extracted with diethyl ether
  7. washThe combined extracts are washed with water
  8. dry with materialdried over sodium sulfate
  9. concentrationconcentrated under reduced pressure
  10. customThe residue is purified
  11. customto give the product