HRID1081320

反应详情

EQUATION

反应方程式

HRID 1081320 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 6-[N-[3,5-bis(trifluoromethyl)benzyl]-N-methylaminocarbonyl]-5-(4-fluorophenyl)-7,8-dihydro-1,7-dimethyl-8-oxopyrido[3,4-b]pyridinium iodide (Example 29) (100 mg), THF (3 ml), potassium ferricyanide (500 mg) and 1N-NaOH was stirred for 15 hours. The solvent was distilled off. To the residue was added ethyl acetate, and the mixture was washed with water and dried, then the solvent was distilled off. The residue was subjected to a silica-gel column chromatography (ethyl acetate) for separation and purification to afford the above-titled compound as colorless crystals (35 mg), m.p.210°-212° C. (recrystallized from ethyl acetate-isopropyl ether).

WORKUP

后处理

  1. distillationThe solvent was distilled off
  2. additionTo the residue was added ethyl acetate
  3. washthe mixture was washed with water
  4. customdried
  5. distillationthe solvent was distilled off
  6. customThe residue was subjected to a silica-gel column chromatography (ethyl acetate) for separation and purification
  7. customto afford
  8. customthe above-titled compound as colorless crystals (35 mg), m.p.210°-212° C. (recrystallized from ethyl acetate-isopropyl ether)