反应详情

3-Ethyl-2-naphthalen-1-yl-3H-imidazole-4-carboxylic acid (105 mg, 0.394 mmol) and 1-cyclobutylpiperazine bistrifluoroacetate (145 mg, 0.394 mmol, 1.0 eq.) are dissolved in DCM (5 ml), and to the solution is added Et3N (4 eq.), followed by BOP coupling regent (183 mg, 0.433 mmol, 1.1 eq.). The resulting mixture is stirred at rt overnight. DCM is evaporated, and the residue is taken up in EtOAc (1.0 ml). The solution is washed thoroughly with water (3.0 ml×3) to remove the by-product from BOP, and then washed with brine. The solution is dried over sodium sulfate, concentrated and purified through PTLC to give the title compound. 1H NMR (300 MHz, CDCl3) δ 7.98 (1H, m), 7.92 (1H, dd), 7.44˜7.63 (5H, m), 7.39 (1H, s), 4.05 (2H, q), 3.89 (4H, s, br), 2.80 (1H, m), 2.43 (4H, s, br), 1.50˜2.20 (6H, m), 1.09 (3H, t); LCMS 389 (M+1).

1. customDCM is evaporated
2. washThe solution is washed thoroughly with water (3.0 ml×3)
3. customto remove the by-product from BOP
4. washwashed with brine
5. dry with materialThe solution is dried over sodium sulfate
6. concentrationconcentrated
7. custompurified through PTLC