HRID1079304

反应详情

EQUATION

反应方程式

HRID 1079304 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 3-(2-hydroxybenzoyl)acrylic acid (3.02 g) in aqueous sodium carbonate (5%, 55 ml) was stirred at room temperature for 15 hours, acidified with 2N HCl and extracted with ethyl acetate. The ethyl acetate layer was washed with water, dried (MgSO4) and then treated with activated charcoal, after which the solvent was distilled off, to yield 2,3-dihydro-4-oxo-4H-1-benzopyran-2-carboxylic acid (2.01 g, 67%), which was then recrystallized from ethyl acetate-hexane to yield colorless prisms having a melting point of 170° to 171° C.

WORKUP

后处理

  1. extractionextracted with ethyl acetate
  2. washThe ethyl acetate layer was washed with water
  3. dry with materialdried (MgSO4)
  4. additiontreated with activated charcoal
  5. distillationafter which the solvent was distilled off