HRID652505

反应详情

EQUATION

反应方程式

HRID 652505 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2.91 g of 1-(2,4-dihydroxy-3-propylphenyl) ethanone, 2.91 g of ethyl 4-bromobutyrate and 3.1 g of anhydrous potassium carbonate in 35 ml of anhydrous dimethyl formamide was stirred and heated at 75° for 12 hours. The solvent was removed in vacuo, the residue was treated with water and the product was extracted with ethyl acetate. The dried (over magnesium sulfate) extract was concentrated in vacuo and the crude product was purified by chromatography on 200 g of silica gel. Elution with 5% ethyl acetate-toluene gave 2.55 g (54% yield) of 4-(4-acetyl-3-hydroxy-2-propylphenoxy) butanoic acid ethyl ester, the titled compound, as an oil.

WORKUP

后处理

  1. temperatureheated at 75° for 12 hours
  2. customThe solvent was removed in vacuo
  3. additionthe residue was treated with water
  4. extractionthe product was extracted with ethyl acetate
  5. dry with materialThe dried (over magnesium sulfate)
  6. extractionextract
  7. concentrationwas concentrated in vacuo
  8. customthe crude product was purified by chromatography on 200 g of silica gel
  9. washElution with 5% ethyl acetate-toluene