反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureRefluxing
- stirringwith stirring
- waitThe reaction mixture was kept standing overnight
- customThe precipitate formed
- filtrationwas filtered off
- dissolutiondissolved in 3 liter of diethyl ether
- washThis solution was washed with a saturated sodium chloride solution
- dry with materialdried over sodium sulphate
- concentrationconcentrated
- customThe residue was crystallised from a mixture of methanol and diethyl ether