HRID2418360

反应详情

EQUATION

反应方程式

HRID 2418360 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2-oxo-7-benzyloxyindoline (2.15 g.), sodium hydroxide (0.84 g.), dioxane (20 ml.) and water (20 ml.) was refluxed under heating for 72 hours with stirring. After cooling, the reaction mixture was evaporated under reduced pressure. The residue was dissolved in water and the solution was washed with ethyl acetate. Diethyl ether was added to the solution and adjusted to pH 4 to 5 with 5% sulfuric acid. The diethyl ether layer was separated, washed with water, dried over magnesium sulfate and then evaporated under reduced pressure. The residue was crystallized with a mixture of ethyl acetate and n-hexane to give 2-(2-amino-3-benzyloxyphenyl)acetic acid (2.2 g.).

WORKUP

后处理

  1. temperaturewas refluxed
  2. temperatureunder heating for 72 hours
  3. temperatureAfter cooling
  4. customthe reaction mixture was evaporated under reduced pressure
  5. dissolutionThe residue was dissolved in water
  6. washthe solution was washed with ethyl acetate
  7. additionDiethyl ether was added to the solution
  8. customThe diethyl ether layer was separated
  9. washwashed with water
  10. dry with materialdried over magnesium sulfate
  11. customevaporated under reduced pressure
  12. customThe residue was crystallized with a mixture of ethyl acetate and n-hexane