HRID229733

反应详情

EQUATION

反应方程式

HRID 229733 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a pyridine solution (2 mL) of 7-methyl-3-(3-trifluoromethylphenyl)cinnolin-5-ol (60 mg, 0.2 mmol) obtained in Example 70 was added acetic anhydride (3 mL), followed by reaction at room temperature over night. The reaction liquid was concentrated under reduced pressure, followed by 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 (25 mg, 36%) as pale yellow solid.

WORKUP

后处理

  1. customfollowed by reaction at room temperature over night
  2. customThe reaction liquid
  3. concentrationwas concentrated under reduced pressure
  4. additionby adding
  5. distillationdistilled
  6. extractionwater (1 mL), extraction
  7. customwith ethyl acetate and purification of residue
  8. customobtained after concentration of an organic layer under reduced pressure