HRID2211187

反应详情

EQUATION

反应方程式

HRID 2211187 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a suspension of 2-[(2,6-dichloro-3-methylphenyl)amino]-benzoic acid hydrazide (394.1 mg, 1.27 mmoles) in 20 ml of 2-propanol is added triethylamine (200 μl, 1.43 mmoles) followed by diphenyl cyanocarbonimidate (371.9 mg, 1.56 mmoles). After 1.5 hours the resultant yellow solution is concentrated in vacuo. The residue is dissolved in 10 ml of ethyl acetate and partitioned between water and a 1:1 mixture of ether and hexane. The aqueous layer is acidified with 1N hydrochloric acid, and the resultant white solid is collected by filtration to provide 99.3 mg (22%) of 5-[2-[(2,6-dichloro-3-methylphenyl)amino]phenyl]-1,3,4-oxadiazol-2-yl-cyanamide, mp above 215° C.

WORKUP

后处理

  1. concentrationAfter 1.5 hours the resultant yellow solution is concentrated in vacuo
  2. dissolutionThe residue is dissolved in 10 ml of ethyl acetate
  3. custompartitioned between water
  4. additiona 1:1 mixture of ether and hexane
  5. filtrationthe resultant white solid is collected by filtration