HRID328115

反应详情

EQUATION

反应方程式

HRID 328115 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureThis mixture is then refluxed for one hour
  2. temperaturecooled slightly
  3. temperatureThe reaction mixture is refluxed for 18 hours
  4. temperatureThe resulting residue is cooled
  5. filtrationfiltered
  6. customto remove a small amount of solid
  7. customThe filtrate is evaporated in vacuo
  8. dissolutionthe resulting oil is dissolved in ether
  9. washwashed with water, 10 percent sodium carbonate, water
  10. dry with materialThe ether solution is dried over anhydrous magnesium sulfate
  11. filtrationfiltered
  12. customto remove the charcoal
  13. customthe filtrate evaporated in vacuo