HRID1244984

反应详情

EQUATION

反应方程式

HRID 1244984 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

0.83 g (9.58 mmol) of O-methylhydroxylamine hydrochloride and 1.56 ml (11.2 mmol) of triethylamine were added to a solution of 0.85 mg (3.2 mmol) of 2-(4-fluorophenyl)-4-formyl-3-(pyridin-4-yl)-1H-pyrrole [prepared as described in Example 1(iii) above] in 17 ml of methanol. The resulting mixture was heated under reflux for 30 minutes, after which water was added to the reaction mixture which was then extracted with ethyl acetate. The organic extract was washed with water and concentrated by evaporation under reduced pressure. The resulting residue was purified by chromatography on a silica gel column using ethyl acetate as the eluant to afford 728 mg (yield 77%) of the title compound as a pale yellow powder.

WORKUP

后处理

  1. temperatureThe resulting mixture was heated
  2. temperatureunder reflux for 30 minutes
  3. extractionwas then extracted with ethyl acetate
  4. extractionThe organic extract
  5. washwas washed with water
  6. concentrationconcentrated by evaporation under reduced pressure
  7. customThe resulting residue was purified by chromatography on a silica gel column