HRID622403

反应详情

EQUATION

反应方程式

HRID 622403 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

25.6 g (0.1 mole) of 1-(2,4-dichlorophenyl)-2-(1,2,4-triazol-1-yl)-1-ethanone are dissolved in 610 ml of methanol, and 6.3 g (0.15 mole) of sodium borohydride are added in portions at 5° to 10° C., while stirring. The mixture is then stirred at room temperature for one hour and heated at the boil for one hour. After the solvent has been distilled off, 250 ml of water and 50 ml of concentrated hydrochloric acid are added to the residue and the mixture is boiled up for 15 minutes. After the reaction mixture has been rendered alkaline with sodium hydroxide solution, the solid reaction product can be filtered off. It is recrystallized from aqueous acetonitrile. 12 g (42% of theory) of 1-(2,4-dichlorophenyl)-2-(1,2,4-triazol-1-yl)-1-ethanol of melting point 87° C. are obtained.

WORKUP

后处理

  1. stirringThe mixture is then stirred at room temperature for one hour
  2. temperatureheated at the boil for one hour
  3. distillationAfter the solvent has been distilled off
  4. addition250 ml of water and 50 ml of concentrated hydrochloric acid are added to the residue
  5. customthe solid reaction product
  6. filtrationcan be filtered off
  7. customIt is recrystallized from aqueous acetonitrile