HRID1256182

反应详情

EQUATION

反应方程式

HRID 1256182 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4.43 g (21.2 mmol, 1 eq) of 3-bromo-1,5-naphthyridine (W. Czuba, Recueil des Travaux Chimiques des Pays-Bas 1963, 82, 988-996) were introduced in 165 mL of methylene chloride. 5.23 g (21.2 mmol, 1 eq) of meta-chloroperbenzoic acid were then added portionwise at 0° C. The mixture was stirred at rt for 18 h. The mixture was washed with 1M aqueous NaOH solution and water. Organic layer was dried over Na2SO4, filtered and evaporated to dryness. The residue was purified by column chromatography using methylene chloride and then methylene chloride/ethanol: 98/2 as eluent. The solvent was evaporated to dryness to afford 3.08 g of 3-bromo-1,5-naphthyridine-5-oxide (pale yellow powder) with 64% yield and 1.00 g of 3-bromo-1,5-naphthyridine-1-oxide (yellow powder) with 21% yield.

WORKUP

后处理

  1. washThe mixture was washed with 1M aqueous NaOH solution and water
  2. dry with materialOrganic layer was dried over Na2SO4
  3. filtrationfiltered
  4. customevaporated to dryness
  5. customThe residue was purified by column chromatography
  6. customThe solvent was evaporated to dryness