HRID261975

反应详情

EQUATION

反应方程式

HRID 261975 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 19.2 g of α,α-bis(p-chlorophenyl)imidazole-2-methanol (prepared according to Example III B) and 3 g of sodium hydroxyde in 250 ml. of acetonitrile was refluxed for one hour with stirring. Then 500 mg of picric acid, a few crystals of potassium iodide and a solution of 11.3 g of benzyl bromide in 100 ml. of acetonitrile were added. Refluxing was then continued for 4 hours with stirring. The reaction mixture was kept standing overnight. The precipitate formed was filtered off and dissolved in 3 liter of diethyl ether. This solution was washed with a saturated sodium chloride solution, decolorized with active charcoal, dried over sodium sulphate and concentrated. The residue was crystallised from a mixture of methanol and diethyl ether. 1-Benzyl-α,α-bis(p-chlorophenyl)imidazole-2-methanol was obtained. Melting point 167°-168° C.

WORKUP

后处理

  1. temperatureRefluxing
  2. stirringwith stirring
  3. waitThe reaction mixture was kept standing overnight
  4. customThe precipitate formed
  5. filtrationwas filtered off
  6. dissolutiondissolved in 3 liter of diethyl ether
  7. washThis solution was washed with a saturated sodium chloride solution
  8. dry with materialdried over sodium sulphate
  9. concentrationconcentrated
  10. customThe residue was crystallised from a mixture of methanol and diethyl ether