HRID2268509

反应详情

EQUATION

反应方程式

HRID 2268509 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 7-(2-iodoethyl)-1,2,3,4-tetramethoxy-6,7,8,9-tetrahydro-5H-benzo[a]cycloheptene (1.50 g), 2-quinolinol (621 mg), and potassium carbonate (987 mg) in DMF (15 ml) was stirred at room temperature for 12 hr. After being stirred at 60° C. for 6 hr, the reaction mixture was diluted with water and extracted with ethyl acetate. The organic layer was washed with water and saturated aqueous sodium chloride and dried. The solvent was removed in vacuo. The residue was diluted with dilsopropylether. The crystals were collected by filtration and recrystallized from hexane-ethyl acetate to obtain 2-[2-(1,2,3,4-tetramethoxy-6,7,8,9-tetrahydro-5H-benzo[a]cyclohepten-7-yl)ethoxy]quinoline (680 mg).

WORKUP

后处理

  1. stirringAfter being stirred at 60° C. for 6 hr
  2. extractionextracted with ethyl acetate
  3. washThe organic layer was washed with water and saturated aqueous sodium chloride
  4. customdried
  5. customThe solvent was removed in vacuo
  6. additionThe residue was diluted with dilsopropylether
  7. filtrationThe crystals were collected by filtration
  8. customrecrystallized from hexane-ethyl acetate