HRID703171
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
75 ml of acetic anhydride were added dropwise at room temperature to a solution of 31,3 g of 4-ethoxy-2,3,5-trimethylpyridine 1-oxide in 100 ml of chloroform. After boiling under reflux for 16 hours the solution was evaporated, the residue was dissolved in 100 ml of toluene and again evaporated. The residue was taken up in 250 ml of ethyl acetate, whereupon it was extracted three times with 100 ml of saturated sodium bicarbonate solution. The organic phase was dried over sodium sulfate and evaporated in vacuo. The product was chromatographed on 170 g of silica gel with ether. There was obtained (4-ethoxy-3,5-dimethyl-2-pyridyl)methyl acetate in the form of an oil.
WORKUP
后处理
- temperatureunder reflux for 16 hours the solution
- customwas evaporated
- dissolutionthe residue was dissolved in 100 ml of toluene
- customagain evaporated
- extractionwas extracted three times with 100 ml of saturated sodium bicarbonate solution
- dry with materialThe organic phase was dried over sodium sulfate
- customevaporated in vacuo
- customThe product was chromatographed on 170 g of silica gel with ether