HRID327528

反应详情

EQUATION

反应方程式

HRID 327528 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

In a round bottomed flask, 2.2 mmol of 3-amino-5-methoxychroman (described in Patent EP 279,150) are dissolved in 6 ml of dimethylformamide in the presence of 2.4 mmol of N-(4-bromobutyl)phthalimide, 6.6 mmol of potassium carbonate and a catalytic amount of potassium iodide. The mixture is left stirring at 60° C. for 6 hours. After cooling, the solvent is evaporated off and, after aqueous hydrolysis, the crude reaction mixture is extracted with dichloromethane. After washing, drying and evaporation of the organic phase, the expected product is obtained after purification by chromatography on a silica column (elution solvent: ether/petroleum ether, 5:95).

WORKUP

后处理

  1. waitThe mixture is left
  2. temperatureAfter cooling
  3. customthe solvent is evaporated off
  4. customafter aqueous hydrolysis
  5. customthe crude reaction mixture
  6. extractionis extracted with dichloromethane
  7. washAfter washing
  8. customdrying
  9. customevaporation of the organic phase