HRID31428

反应详情

EQUATION

反应方程式

HRID 31428 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A solution of sodium azide (14.8 mg) in water (1.25 ml) was added to 4′-[5-(chloromethyl)-1,3,4-oxadiazol-2-yl]-N-cyclopropyl-6-methyl-1,1′-biphenyl-3-carboxamide (Intermediate 45) (40 mg) in DMF (0.5 ml) and ethanol (2.5 ml) and the mixture heated at reflux for 2 hours. The solvents were evaporated under vacuum and the residue partitioned between water (20 ml) and chloroform (15 ml). The aqueous was extracted with chloroform (15 ml) and the combined organic phases dried (sodium sulphate) and reduced to dryness in vacuo to give 4′-[5-(azidomethyl)-1,3,4-oxadiazol-2-yl]-N-cyclopropyl-6-methyl-1,1′-biphenyl-3-carboxamide,

WORKUP

后处理

  1. temperaturethe mixture heated
  2. temperatureat reflux for 2 hours
  3. customThe solvents were evaporated under vacuum
  4. customthe residue partitioned between water (20 ml) and chloroform (15 ml)
  5. extractionThe aqueous was extracted with chloroform (15 ml)
  6. dry with materialthe combined organic phases dried (sodium sulphate)