HRID653704

反应详情

EQUATION

反应方程式

HRID 653704 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of methyl 3-valerylaminobenzoate (2.3 g) in acetic anhydride (12 ml) was added dropwise fuming nitric acid (1.4 ml) while stirring under ice-cooling. To the mixture was added one drop of conc. sulfuric acid and the mixture was stirred for two hours. To the reaction mixture was added ice-water and it was extracted with ethyl acetate. The organic layer was washed with an aqueous solution of sodium bicarbonate and water and then dried. The solvent was evaporated to dryness, and the residue was purified by column chromatography on silica gel to afford a brown oil (1.0 g, 36%).

WORKUP

后处理

  1. temperaturecooling
  2. stirringthe mixture was stirred for two hours
  3. extractionwas extracted with ethyl acetate
  4. washThe organic layer was washed with an aqueous solution of sodium bicarbonate and water
  5. customdried
  6. customThe solvent was evaporated to dryness
  7. customthe residue was purified by column chromatography on silica gel