HRID13244

反应详情

EQUATION

反应方程式

HRID 13244 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

92 mg of OXONE and 0.1 ml of water were added to a tetrahydrofuran (1.5 ml) solution of 42 mg of 5-(2-methyl-pyridin-5-ylsulfanyl)-2-pyridin-2-yl-6-(pyridin-3-yloxy)-1H-benzimidazole obtained in Example 13, and the reaction liquid was stirred overnight at room temperature. The solvent was evaporated away 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]. An aqueous solution of saturated sodium hydrogencarbonate was added to the resulting fraction, and this was extracted with chloroform, and dried with anhydrous magnesium sulfate. The solvent was evaporated away under reduced pressure to obtain the entitled compound.

WORKUP

后处理

  1. customthe reaction liquid
  2. customThe solvent was evaporated away under reduced pressure
  3. 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]
  4. additionAn aqueous solution of saturated sodium hydrogencarbonate was added to the resulting fraction
  5. extractionthis was extracted with chloroform
  6. dry with materialdried with anhydrous magnesium sulfate
  7. customThe solvent was evaporated away under reduced pressure
  8. customto obtain the entitled compound