HRID1448405

反应详情

EQUATION

反应方程式

HRID 1448405 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution was prepared by dissolving 6.9 grams (0.3 mole) of sodium metal in 700 milliliters of 95 percent ethanol. To this solution was added with stirring 54.5 grams (0.3 mole) of 3,5-dichloro-6-fluoro-2-pyridinol. Thereafter 58.5 grams (0.35 mole) of ethyl bromoacetate was added and the mixture refluxed for 5 hours. At the completion of the reaction, the ethanol was distilled off and the residue poured into water. The solid which precipitated was filtered off and taken up in hexane and dried with activated carbon and anhydrous sodium sulfate. The mixture was filtered and the hexane removed and the ethyl-(3,5-dichloro-6-fluoro-2-pyridyloxy) acetate product was recovered by distillation. The product was a white waxy solid which boiled at 135°-170° C. (M.P. 63.5°-64° C.)

WORKUP

后处理

  1. customA solution was prepared
  2. additionTo this solution was added
  3. temperaturethe mixture refluxed for 5 hours
  4. customAt the completion of the reaction
  5. distillationthe ethanol was distilled off
  6. additionthe residue poured into water
  7. customThe solid which precipitated
  8. filtrationwas filtered off
  9. dry with materialdried with activated carbon and anhydrous sodium sulfate
  10. filtrationThe mixture was filtered
  11. customthe hexane removed
  12. distillationthe ethyl-(3,5-dichloro-6-fluoro-2-pyridyloxy) acetate product was recovered by distillation