HRID1084750

反应详情

EQUATION

反应方程式

HRID 1084750 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
25 °C

PROCEDURE

实验过程

6.5 g of 2,8-dihydroxyquinoline, 5.5 g of anhydrous ground potassium carbonate are stirred in 100 ml of dimethylformamide at 25° C. for 1 hour. After addition of 13.1 g of 1-(2-bromomethylphenyl)heptyl acetate in 50 ml of dimethylformamide, the mixture is stirred at 25° C. for 20 hours. The solvent is removed in vacuo, the residue is taken up in 100 ml of water and the mixture is extracted 3 times with 50 ml of ethyl acetate each time. The organic phases are washed once with 50 ml of water each time, dried over Na2SO4 and concentrated in vacuo. The oil which remains is chromatographed over silica gel 60 with CH2Cl2 /ethyl acetate 10:1. The resulting product slowly crystallizes out.

WORKUP

后处理

  1. customThe solvent is removed in vacuo
  2. extractionthe mixture is extracted 3 times with 50 ml of ethyl acetate each time
  3. washThe organic phases are washed once with 50 ml of water each time
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated in vacuo
  6. customThe oil which remains is chromatographed over silica gel 60 with CH2Cl2 /ethyl acetate 10:1
  7. customThe resulting product slowly crystallizes out