反应详情

A mixture of 1-(2-tert-butylphenyl)piperazine dihydrochloride (Reference Example 1, 1.63 g, 5.60 mmol), 2-methyl-1H-imidazole-4-carboxylic acid (1.0 g, 6.16 mmol), triethylamine (3.12 mL, 22.4 mmol), EDCI (0.96 g, 6.16 mmol) and HOBt (0.94 g, 6.16 mmol) in N,N-dimethylformamide (20 mL) was stirred at room temperature for 16 h. To the reaction mixture was added saturated NaHCO3 solution and extracted with ethyl acetate. The extract was washed with saturated NaHCO3 solution, 1 M HCl and brine, dried over anhydrous magnesium sulfate, filtered and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (hexane/ethyl acetate 98:2 to 75:25) to give the title compound (1.63 g, 89%) as a white solid.

1. extractionextracted with ethyl acetate
2. washThe extract was washed with saturated NaHCO3 solution, 1 M HCl and brine
3. dry with materialdried over anhydrous magnesium sulfate
4. filtrationfiltered
5. concentrationconcentrated under reduced pressure
6. customThe residue was purified by silica gel column chromatography (hexane/ethyl acetate 98:2 to 75:25)