HRID229734

反应详情

EQUATION

反应方程式

HRID 229734 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To an acetone solution (5 mL) of 7-methyl-3-(3-trifluoromethylphenyl)cinnolin-5-ol (69 mg, 0.2 mmol) obtained in Example 70 were added benzyl bromide (0.024 mL) and potassium carbonate (28 mg, 0.2 mmol), followed by stirring at room temperature over night and refluxing under heating for 3 hours. The reaction liquid was further added with benzyl bromide (0.024 mL) and potassium carbonate (28 mg, 0.2 mmol), followed by stirring at room temperature over night, concentration of the reaction liquid under reduced pressure, adding distilled water (1 mL), extraction with ethyl acetate and purification of residue obtained after concentration of an organic layer under reduced pressure, with HPLC column chromatography (hexane/ethyl acetate=3/1) to obtain an objective compound (8 mg, 10%).

WORKUP

后处理

  1. temperaturerefluxing
  2. temperatureunder heating for 3 hours
  3. customThe reaction liquid
  4. stirringby stirring at room temperature over night
  5. customconcentration of the reaction liquid under reduced pressure
  6. additionadding
  7. distillationdistilled
  8. extractionwater (1 mL), extraction
  9. customwith ethyl acetate and purification of residue
  10. customobtained after concentration of an organic layer under reduced pressure