HRID1703444

反应详情

EQUATION

反应方程式

HRID 1703444 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 19.7 parts of 4-chloro-2-fluorophenylhydrazine and 14.0 parts of 2-acetylcyclohexanone in 50 parts of xylene and 1 part of glacial acetic acid were refluxed for 24 hours with a Dean Stark trap to collect the water formed. The xylene was distilled from the mixture. The residual oil was dissolved in arm hexane solution. On cooling, 6.2 parts of crude product was obtained. Recrystallization of this product yielded white crystals of 2-(4-chloro-2-fluorophenyl)-3-methyl-4,5,6,7-tetrahydro-2H-indazole, melting point 84.5°-87.5° C; ir bands (1570 cm-1, 905 cm-1, 822 cm-1).

WORKUP

后处理

  1. customto collect the water
  2. customformed
  3. distillationThe xylene was distilled from the mixture
  4. dissolutionThe residual oil was dissolved in arm hexane solution
  5. temperatureOn cooling
  6. custom6.2 parts of crude product was obtained
  7. customRecrystallization of this product