HRID483519

反应详情

EQUATION

反应方程式

HRID 483519 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1-[1-(4-Formylbenzoyl)-4-piperidinyl]-3,4-dihydrocarbostyril (1 g), hydroxylamine hydrochloride (580 mg) and sodium acetate (1.6 g) are dissolved in ethanol (20 ml) and water (10 ml) and the mixture is stirred at room temperature overnight. The solvent is concentrated and water is added to the residue. The mixture is extracted with chloroform, dried with sodium carbonate. The solvent is distilled off and the resulting residue is purified by silica gel column chromatography (solvent: n-hexane:ethyl acetate=1:2) and recrystallized from n-hexane/ethanol to give 1-[1-(4-hydroxyiminomethylbenzoyl)-4-piperidinyl]-3,4-dihydrocarbostyril (1 g) as white powder, m.p.: 222°-224° C.

WORKUP

后处理

  1. concentrationThe solvent is concentrated
  2. additionwater is added to the residue
  3. extractionThe mixture is extracted with chloroform
  4. dry with materialdried with sodium carbonate
  5. distillationThe solvent is distilled off
  6. customthe resulting residue is purified by silica gel column chromatography (solvent: n-hexane:ethyl acetate=1:2)
  7. customrecrystallized from n-hexane/ethanol