HRID971644

反应详情

EQUATION

反应方程式

HRID 971644 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred mixture of 19 parts of 1H-1,2,4-triazole and 225 parts of N,N-dimethylformamide are added 8.4 parts of sodium hydride dispersion 78% and stirring is continued till foaming has ceased. Then there are added 29 parts of 1-(2-bromo-1,1-dimethoxyethyl)-2,4-dichlorobenzene and the whole is stirred and refluxed overnight. The reaction mixture is cooled, poured onto water and the product is extracted twice with 2,2'-oxybispropane. The combined extracts are washed with water, dried, filtered and evaporated. The residue is crystallized from petroleumether (activated charcoal), yielding 12.1 parts (44%) of 1-[2-(2,4-dichlorophenyl)-2,2-dimethoxyethyl]-1H-1,2,4-triazole; mp. 87.7° C.

WORKUP

后处理

  1. stirringthe whole is stirred
  2. temperaturerefluxed overnight
  3. temperatureThe reaction mixture is cooled
  4. additionpoured onto water
  5. extractionthe product is extracted twice with 2,2'-oxybispropane
  6. washThe combined extracts are washed with water
  7. customdried
  8. filtrationfiltered
  9. customevaporated
  10. customThe residue is crystallized from petroleumether (activated charcoal)