HRID261960

反应详情

EQUATION

反应方程式

HRID 261960 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 10 g (0.023 mol) of α,α-bis(2,4-dichlorophenyl)-1-(methoxymethyl)imidazole-2-methanol in 150 ml. of glacial acetic acid, 15 ml. of concentrated hydrochloric acid and 15 ml. of water was refluxed for two hours and then concentrated. The residue was dissolved in a small amount of a mixture of ethanol and 2N hydrochloric acid and the solution was extracted with diethyl ether. The extract was dried over sodium sulphate and the ether was distilled off. Diethyl ether and petroleum ether (boiling range 60°-80° C.) were added, the solid substance was filtered off and twice crystallised from isopropyl alcohol with a little ethanol. α,α-Bis(2,4-dichlorophenyl)imidazole-2-methanol was obtained. Melting point 193° C.

WORKUP

后处理

  1. concentrationconcentrated
  2. dissolutionThe residue was dissolved in a small amount of a mixture of ethanol and 2N hydrochloric acid
  3. extractionthe solution was extracted with diethyl ether
  4. dry with materialThe extract was dried over sodium sulphate
  5. distillationthe ether was distilled off
  6. additionDiethyl ether and petroleum ether (boiling range 60°-80° C.) were added
  7. filtrationthe solid substance was filtered off
  8. customtwice crystallised from isopropyl alcohol with a little ethanol