HRID1076351

反应详情

EQUATION

反应方程式

HRID 1076351 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 40 g. (0.27 mole) of crude phenylacetamide oxime in 200 ml. of dry toluene is treated with 45.9 g. (0.27 mole) of chloroacetic anhydride in 100 ml. of toluene. The resultant mixture is then refluxed and the water formed is removed by means of a Dean Stark trap. The mixture is refluxed for 3-4 hours after which it is cooled and extracted once with 150 ml. of water and four times with 100 ml. of a saturated sodium bicarbonate solution. The toluene solution is then dried over magnesium sulfate and the solvent is removed in vacuo. Upon distillation of the residue, 3-benzyl-5-chloromethyl-1,2,4-oxadiazole, 19.8 g. having a b.p. of 100-108 (0.04 mm) is obtained.

WORKUP

后处理

  1. customis removed by means of a Dean Stark trap
  2. temperatureThe mixture is refluxed for 3-4 hours after which it
  3. temperatureis cooled
  4. extractionextracted once with 150 ml
  5. dry with materialThe toluene solution is then dried over magnesium sulfate
  6. customthe solvent is removed in vacuo
  7. distillationUpon distillation of the residue, 3-benzyl-5-chloromethyl-1,2,4-oxadiazole, 19.8 g
  8. customof 100-108 (0.04 mm) is obtained