HRID13359

反应详情

EQUATION

反应方程式

HRID 13359 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

0.005 ml of acetic anhydride was added to a pyridine (1 ml) solution of 13.7 mg of 1-(2-(6-(6-amino-pyridin-3-yloxy)-2-pyridin-2-yl-3H-benzimidazol-5-yl)-pyrrolidin-1-yl)-ethanone, and the reaction liquid was stirred at room temperature for 3 hours. The reaction liquid was evaporated away under reduced pressure, the resulting residue was dissolved in 1 ml of trifluoroacetic acid, and the reaction liquid was stirred at room temperature for 3 hours. The reaction liquid was distilled under reduced pressure, and the resulting residue was purified through reversed-phase middle-pressure liquid chromatography [ODS-AS-360-CC (by YMC), mobile phase: water-acetonitrile-0.1% trifluoroacetic acid] and through silica gel column chromatography (developing solvent: chloroform/methanol=9/1) to obtain the entitled compound as an oily substance.

WORKUP

后处理

  1. customthe reaction liquid
  2. customThe reaction liquid
  3. customwas evaporated away under reduced pressure
  4. dissolutionthe resulting residue was dissolved in 1 ml of trifluoroacetic acid
  5. customthe reaction liquid
  6. stirringwas stirred at room temperature for 3 hours
  7. customThe reaction liquid
  8. distillationwas distilled under reduced pressure
  9. customthe resulting residue was purified through reversed-phase middle-pressure liquid chromatography [ODS-AS-360-CC (by YMC), mobile phase: water-acetonitrile-0.1% trifluoroacetic acid] and through silica gel column chromatography (developing solvent: chloroform/methanol=9/1)
  10. customto obtain the entitled compound as an oily substance