反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
2.19 g (0.09 gr.at.) of magnesium and 10.9 g (0.1 mol) of ethyl bromide were converted into a Grignard compound in 50 ml. of refluxing anhydrous tetrahydrofuran. In the course of 5 minutes a solution of 8.46 g (0.09 mol) of 1-vinylimidazole in 20 ml. of anhydrous tetrahydrofuran was added with stirring to the refluxing mixture, after which the reaction mixture was refluxed for another two hours. A suspension of 22.6 g (0.09 mol) of 4,4'-dichlorobenzophenone in 50 ml. of anhydrous tetrahydrofuran was then added and refluxing was continued for 24 hours. The whole procedure was carried out under a nitrogen atmosphere. After cooling, the reaction mixture was poured into a mixture of ice, water and ammonium chloride. The mixture was then extracted with diethyl ether and the extract was washed with water, dried over sodium sulphate and concentrated. The solid residue was twice crystallized from a mixture of isopropyl alcohol and dimethyl formamide. α,α-Bis(p-chlorophenyl)-1-vinylimidazole-2-methanol was obtained. Melting point 173.5°- 174° C.
WORKUP
后处理
- customIn the course of 5 minutes
- temperatureafter which the reaction mixture was refluxed for another two hours
- temperaturerefluxing
- temperatureAfter cooling
- extractionThe mixture was then extracted with diethyl ether
- washthe extract was washed with water
- dry with materialdried over sodium sulphate
- concentrationconcentrated
- customThe solid residue was twice crystallized from a mixture of isopropyl alcohol and dimethyl formamide