HRID2090541

反应详情

EQUATION

反应方程式

HRID 2090541 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Further, in a nitrogen atmosphere, 3′,5′-bis(trifluoromethyl)-2-aminobenzophenone (1.1 g, 3.3 mmol) was dissolved in toluene (13 mL), and acetic anhydride (0.62 mL, 6.5 mL) was added to the solution at room temperature, followed by stirring while heating and refluxing. The mixture was cooled to room temperature and then concentrated using a rotary evaporator. The residue was dissolved in ethylene glycol dimethyl ether (13 mL), and potassium tert-butoxide (1.5 mL, 13 mmol) was added to the solution at room temperature, followed by stirring for 2 hours. Water was added to the reaction solution, followed by extraction with methylene chloride. The organic layer was dried and then concentrated using a rotary evaporator. The residue was purified by silica gel column chromatography (hexane/ethyl acetate). Thus, 4-{3,5-bis(trifluoromethyl)phenyl}-2-quinolinone (372 mg, 1.04 mmol) was obtained in a yield of 32%.

WORKUP

后处理

  1. temperaturewhile heating
  2. temperaturerefluxing
  3. concentrationconcentrated
  4. customa rotary evaporator
  5. dissolutionThe residue was dissolved in ethylene glycol dimethyl ether (13 mL)
  6. stirringby stirring for 2 hours
  7. extractionfollowed by extraction with methylene chloride
  8. customThe organic layer was dried
  9. concentrationconcentrated
  10. customa rotary evaporator
  11. customThe residue was purified by silica gel column chromatography (hexane/ethyl acetate)