反应详情

A mixture of Compound (7) (6.4 mg, 0.012 mmol) and cis-1,2-cyclopentanedicarboxylic acid (1.9 mg, 0.014 mmol) in pyridine (0.2 mL) was stirred at RT over the weekend. The solvent was removed under pressure. The crude material was purified by preparative LCMS (5-100% ACN in 0.1% aqueous formic acid) to afford Compound (63) as a white solid (0.7 mg, 8%). ESI-MS m/z calculated for [M+H]+: 660.2/662.2; found: 660.0/662.0; 1H NMR (400 MHz, CDCl3) δ 7.93 (s, 0.5H), 7.87 (s, 0.5H), 7.71 (d, J=8.7 Hz, 2H), 7.51 (dd, J=8.8, 2.2 Hz, 2H), 7.40 (d, J=3.7 Hz, 1H), 6.02-5.92 (m, 1H), 5.87 (d, J=4.1 Hz, 1H), 4.05-3.68 (m, 2H), 3.68-3.40 (m, 1H), 3.35-2.95 (m, 3H), 3.21 (s, 3H), 3.05 (d, J=4.9 Hz, 3H), 2.55-2.37 (m, 1H), 2.28-2.11 (m, 1H), 2.10-1.89 (m, 7H), 1.20-0.90 (m, 3H), 0.72-0.47 (m, 1H).

1. customThe solvent was removed under pressure
2. customThe crude material was purified by preparative LCMS (5-100% ACN in 0.1% aqueous formic acid)