HRID2421276

反应详情

EQUATION

反应方程式

HRID 2421276 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customprepared under experimental conditions similar to those previously and
  2. customreagents and reaction products)
  3. additionbefore being poured into ice-
  4. extractionThe mixture is extracted with ethyl acetate
  5. washthe organic phase is washed with water
  6. dry with materialAfter drying over magnesium sulphate
  7. concentrationthe solvents are concentrated
  8. customa rotary evaporator
  9. customAfter purification on a silica column (eluent: ethyl acetate-heptane/7-3)
  10. customa light yellow-coloured solid is obtained in the form of a paste (yield of 13%)