HRID987364

反应详情

EQUATION

反应方程式

HRID 987364 的结构方程式

PROCEDURE

实验过程

3-Methyl-2-hydroxy-5-nonylacetophenone (2b) (102.5 g, 0.37 mol) was treated with hydroxylamine sulfate (36.44 g, 0.22 mol) and anhydrous sodium acetate (36.44 g, 0.44 mol) in methanol (150 mL) at reflux for 7 h. Crude product in the solvent was filtered and concentrated. The resulting oxime was converted to copper(II) complex and purified further by flash column chromatography. Pure fractions were pooled and treated with aqueous 200 gpl sulfuric acid. Removal of the solvent gave 3-methyl-5-nonylsalicylaldoxime.

WORKUP

后处理

  1. temperatureat reflux for 7 h
  2. filtrationCrude product in the solvent was filtered
  3. concentrationconcentrated
  4. custompurified further by flash column chromatography
  5. additiontreated with aqueous 200 gpl sulfuric acid
  6. customRemoval of the solvent