反应详情

To a suspension of 3-chloro-4-((5-(2-(4-chloro-3-methoxyphenyl)propan-2-yl)-1-(4-fluorophenyl)-1H-imidazol-2-ylthio)methyl)-5-fluorobenzoic acid (0.11 g, 0.19 mmol), 1-(2-aminoethyl)-4-aza-1-azoniabicyclo[2.2.2]octane chloride hydrochloride (0.066 g, 2.5 mmol), and HATU (0.088 g, 0.23 mmol) in DMF (0.7 mL) was added DIPEA (0.2 mL, 1.16 mmol). The reaction was stirred for 2 h and purified by HPLC (MeCN/H2O, 10-99%, 0.05% TFA modifier). The product fractions were concentrated and then dissolved in THF (2 mL) and 2N solution of HCl in ether (2 mL). The mixture was filtered to afford the title compound (59 mg) as a white solid. 1H-NMR (DMSO-d6, 400 MHz) δ 9.67 (s, 1H), 7.84 (s, 1H), 7.84-7.76 (m, 2H), 7.27 (d, J=8.2 Hz, 1H), 7.01-6.97 (m, 2H), 6.50-6.43 (m, 4H), 4.22 (s, 2H), 3.86-3.71 (m, 10H), 3.67 (s, 3H), 3.53-3.49 (m, 6H), 1.49 (s, 6H); MS (ES): 700 [M]+.

1. custompurified by HPLC (MeCN/H2O, 10-99%, 0.05% TFA modifier)
2. concentrationThe product fractions were concentrated
3. dissolutiondissolved in THF (2 mL)
4. filtrationThe mixture was filtered