HRID247559

反应详情

EQUATION

反应方程式

HRID 247559 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

5 g of 3-(p-hydroxybenzoyl) indole were dissolved in 50 ml of dimethylformamide containing 2.28 g of sodium methoxide. 4.0 g of 3-chloropropanol was added to the solution followed by stirring at 110° C. in oil bath for 3 hours. After cooling, the solution was concentrated and extracted with 100 ml of ethyl acetate and 50 ml of water. The organic layer obtained was concentrated, and then the residue was purified by column chromatography on silica gel. Crude product was recrystallized from ethyl acetate to give 3-[p-(3-hydroxypropoxy)benzoyl]indole (compound 23) in the form of white needle crystals. (Yield: 30.5%).

WORKUP

后处理

  1. temperatureAfter cooling
  2. concentrationthe solution was concentrated
  3. extractionextracted with 100 ml of ethyl acetate and 50 ml of water
  4. customThe organic layer obtained
  5. concentrationwas concentrated
  6. customthe residue was purified by column chromatography on silica gel
  7. customCrude product was recrystallized from ethyl acetate