反应详情

Carbonyl dimidazole (0.28 g, 1.71 mmol) was added to a solution of α-[[(2,4,6-trimethoxyphenyl)amino]carbonyl]-benzene acetic acid (0.56 g, 1.63 mmol) in dry THF (20 mL), and the resulting mixture was stirred at room temperature for 1 hour, then N-hydroxy-tridecane imidamide (0.37 g, 1.63 mmol) was added, and the mixture stirred for 1.5 hours, concentrated in vacuo, dissolved in glacial acetic acid, and refluxed for 1.5 hours. The solution was concentrated and azeotroped with benzene (2×25 mL), dissolved in ethyl acetate, and washed with NaHCO3, water, brine, dried with MgSO4, and recrystallized from ethanol/water to yield a white solid (0.093 g, 11%). (found): C, 69.25; H, 8.08; N, 7.68. ##STR13##

1. stirringthe mixture stirred for 1.5 hours
2. concentrationconcentrated in vacuo
3. dissolutiondissolved in glacial acetic acid
4. temperaturerefluxed for 1.5 hours
5. concentrationThe solution was concentrated
6. customazeotroped with benzene (2×25 mL)
7. dissolutiondissolved in ethyl acetate
8. washwashed with NaHCO3, water, brine
9. dry with materialdried with MgSO4
10. customrecrystallized from ethanol/water