HRID229732

反应详情

EQUATION

反应方程式

HRID 229732 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 (30.4 mg, 0.1 mmol) obtained in Example 70 were added methyl iodide (0.006 mL, 0.11 mmol) and potassium carbonate (13.8 mg, 0.11 mmol), followed by reaction at room temperature over night. To residue obtained by concentration of the reaction liquid under reduced pressure was added distilled water (1 mL) and extracted with ethyl acetate. Residue obtained after concentration of an organic layer under reduced pressure was purified with silica gel column chromatography (hexane/ethyl acetate=1/1) to obtain an objective compound (5 mg, 15%) as white solid.

WORKUP

后处理

  1. customfollowed by reaction at room temperature over night
  2. customTo residue obtained by concentration of the reaction liquid under reduced pressure
  3. additionwas added
  4. distillationdistilled water (1 mL)
  5. extractionextracted with ethyl acetate
  6. customResidue obtained after concentration of an organic layer under reduced pressure
  7. customwas purified with silica gel column chromatography (hexane/ethyl acetate=1/1)