反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customA solution was prepared
- additionTo this solution was added
- temperaturethe mixture refluxed for 5 hours
- customAt the completion of the reaction
- distillationthe ethanol was distilled off
- additionthe residue poured into water
- customThe solid which precipitated
- filtrationwas filtered off
- dry with materialdried with activated carbon and anhydrous sodium sulfate
- filtrationThe mixture was filtered
- customthe hexane removed
- distillationthe ethyl-(3,5-dichloro-6-fluoro-2-pyridyloxy) acetate product was recovered by distillation