HRID1721925

反应详情

EQUATION

反应方程式

HRID 1721925 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

0.63 g of 2,3-dichloro-4-(1-ethoxymethyl-5-pyrazolylcarbonyl)phenol, 0.58 g of bromoacetic acid and 1.11 g of potassium carbonate are added to 40 ml of acetone, and the mixture is refluxed for 48 hours. The reaction mixture is concentrated to remove solvent, and water is added to the residue. The aqueous mixture is washed with ethyl acetate, acidified with 10% hydrochloric acid and then extracted with ethyl acetate. The extract is washed with a saturated sodium chloride solution, dried and evaporated to remove solvent. The residue is crystallized with water, and the crystals are separated by filtration, washed successively with water and isopropyl ether, and dried to give 0.42 g of [2,3-dichloro-4-(1-ethoxymethyl-5-pyrazolylcarbonyl)phenoxy]acetic acid.

WORKUP

后处理

  1. temperaturethe mixture is refluxed for 48 hours
  2. concentrationThe reaction mixture is concentrated
  3. customto remove solvent, and water
  4. additionis added to the residue
  5. washThe aqueous mixture is washed with ethyl acetate
  6. extractionextracted with ethyl acetate
  7. washThe extract is washed with a saturated sodium chloride solution
  8. customdried
  9. customevaporated
  10. customto remove solvent
  11. customThe residue is crystallized with water
  12. customthe crystals are separated by filtration
  13. washwashed successively with water and isopropyl ether
  14. customdried