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
N-benzyl(4-[1,1′-biphenyl]-4-yl-1H-imidazol-2-yl)methanamine (1 g; 0.0024 mol; prepared under experimental conditions similar to those previously and using suitable starting reagents and reaction products) is diluted in 15 ml of dimethylformamide. Potassium carbonate (1 g; 0.0073 mol) is added at 23° C. then hexane bromide (0.34 ml; 0.0024 mol) is added fairly slowly. The reaction mixture is brought to about 70° C. for 3 hours before being poured into ice-cooled water. The mixture is extracted with ethyl acetate and the organic phase is washed with water. After drying over magnesium sulphate, the solvents are concentrated using a rotary evaporator. After purification on a silica column (eluent: ethyl acetate-heptane/7-3), a light yellow-coloured solid is obtained in the form of a paste (yield of 13%). Free base. Melting point: 120-122° C.
WORKUP
后处理
- customprepared under experimental conditions similar to those previously and
- customreagents and reaction products)
- additionbefore being poured into ice-
- extractionThe mixture is extracted with ethyl acetate
- washthe organic phase is washed with water
- dry with materialAfter drying over magnesium sulphate
- concentrationthe solvents are concentrated
- customa rotary evaporator
- customAfter purification on a silica column (eluent: ethyl acetate-heptane/7-3)
- customa light yellow-coloured solid is obtained in the form of a paste (yield of 13%)