反应详情

温度

60 °C

A solution of 1-[5-bromo-2-nitro-4-(trifluoromethyl)phenyl]-1H-imidazole (580 mg; 1.73 mmol; 1 eq) prepared as in example 52 step 2, benzylamine (210 μl; 1.9 mmol; 1.1 eq) and diisopropylethylamine (331 μl; 1.9 mmol; 1.1 eq) in anhydrous acetonitrile is stirred at 60° C. for 16 h. Concentration, partition (ethyl acetate/aqueous ammonium chloride), extraction of the aqueous phase (ethyl acetate), reunion of the organic phases, drying (magnesium sulfate), concentration and purification by prep CCM on silicagel (dichloromethane/ethyl acetate 50:50) affords the title product (200 mg; 0.552 mmol; 32%) as a yellow solid.

1. concentrationConcentration
2. custompartition
3. extraction(ethyl acetate/aqueous ammonium chloride), extraction of the aqueous phase (ethyl acetate), reunion of the organic phases
4. customdrying
5. concentration(magnesium sulfate), concentration and purification by prep CCM on silicagel (dichloromethane/ethyl acetate 50:50)