HRID341280

反应详情

EQUATION

反应方程式

HRID 341280 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a 0.2 M stirred suspension of the α-carboline derivative (200 mg) in anhydrous CH2Cl2 was added AlCl3 (4.5 equiv.) and bromoacetyl bromide (2.1 equiv.), at room temperature under inert atmosphere. The mixture was stirred at reflux until completion of the reaction (followed by t.l.c.). The resulting mixture was then cautiously quenched at 0° C. with H2O. It was extracted with the mixture of EtOAc/DMF (99:1). The resulting organic layer was washed with NaHCO3 saturated aqueous solution and brine, dried over MgSO4, filtered and solvents were removed under reduced pressure. 2-Bromo-1-(9H-pyrido[2,3-b]indol-6-yl)ethanone was obtained in 61% yield after trituration of the crude product in MeOH and filtration

WORKUP

后处理

  1. customat room temperature
  2. stirringThe mixture was stirred
  3. temperatureat reflux until completion of the reaction (followed by t.l.c.)
  4. customThe resulting mixture was then cautiously quenched at 0° C. with H2O
  5. extractionIt was extracted with the mixture of EtOAc/DMF (99:1)
  6. washThe resulting organic layer was washed with NaHCO3 saturated aqueous solution and brine
  7. dry with materialdried over MgSO4
  8. filtrationfiltered
  9. customsolvents were removed under reduced pressure