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 of 13.6 g. (0.1 mole) benzamide oxime in 625 milliliters dioxane is treated dropwise with 19.8 g. (0.1 mole) 2-chloroformyl benzoic acid methyl ester in 200 milliliters dioxane. This mixture is then refluxed for one hour, cooled slightly and treated with 3.3 milliliters of boron trifluoride etherate. The reaction mixture is refluxed for 18 hours. The resulting residue is cooled and filtered to remove a small amount of solid. The filtrate is evaporated in vacuo and the resulting oil is dissolved in ether, washed with water, 10 percent sodium carbonate, water and then brine. The ether solution is dried over anhydrous magnesium sulfate decolorized with charcoal filtered to remove the charcoal and the filtrate evaporated in vacuo to give o-(3-phenyl-1,2,4-oxadiazol-5-yl)-benzoic acid methyl ester.
WORKUP
后处理
- temperatureThis mixture is then refluxed for one hour
- temperaturecooled slightly
- temperatureThe reaction mixture is refluxed for 18 hours
- temperatureThe resulting residue is cooled
- filtrationfiltered
- customto remove a small amount of solid
- customThe filtrate is evaporated in vacuo
- dissolutionthe resulting oil is dissolved in ether
- washwashed with water, 10 percent sodium carbonate, water
- dry with materialThe ether solution is dried over anhydrous magnesium sulfate
- filtrationfiltered
- customto remove the charcoal
- customthe filtrate evaporated in vacuo