HRID261948

反应详情

EQUATION

反应方程式

HRID 261948 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 9 g. (0.025 mol) of 1-(methoxymethyl)-α-phenyl-α-(p-trifluoromethyl-phenyl)imidazole-2-methanol, 70 ml. of glacial acetic acid, 7 ml. of concentrated hydrochloric acid and 7 ml. of water was refluxed for 3.5 hours. After cooling, the liquid was distilled off and 2 N sodium hydroxide solution and a small amount of ethanol were added to the residue. The alcohol was distilled off and the aqueous phase was extracted with diethyl ether. The ethereal solution was washed with water and dried over sodium sulphate and the solvent was distilled off. The residue was first crystallised from a mixture of toluene and petroleum ether (boiling range 40°-60° C.) and subsequently from isopropyl alcohol. α-Phenyl-α-(p-trifluoromethylphenyl)imidazole-2-methanol was obtained. Melting point 174°-175.5° C.

WORKUP

后处理

  1. additionA mixture of 9 g
  2. temperatureAfter cooling
  3. distillationthe liquid was distilled off
  4. addition2 N sodium hydroxide solution and a small amount of ethanol were added to the residue
  5. distillationThe alcohol was distilled off
  6. extractionthe aqueous phase was extracted with diethyl ether
  7. washThe ethereal solution was washed with water
  8. dry with materialdried over sodium sulphate
  9. distillationthe solvent was distilled off
  10. customThe residue was first crystallised from a mixture of toluene and petroleum ether (boiling range 40°-60° C.) and subsequently from isopropyl alcohol