反应详情

A solution of Example 13 (30 mg, 0.068 mmol), N,N-dimethylaminopyridine (17 mg, 0.137 mmol), and N,N-diisopropylethylamine (0.024 mL, 0.137 mmol) in CH2Cl2 (0.75 mL) was treated at room temperature with acetic anhydride (0.01 mL, 0.103 mmol) and stirred for 5 min. The reaction was then added directly to a RediSep dry loader cartridge and purified by column chromatography (9:1:0.175 M CH2Cl2/MeOH/NH3 in CH2Cl2, 0-50%) to afford the title compound (Example 14). 1H NMR (400 MHz, MeOD) δ 8.53-8.41 (m, 1H), 7.96-7.88 (m, 1H), 7.88-7.77 (m, 1H), 7.50-7.36 (m, 1H), 7.31-7.13 (m, 2H), 6.91-6.60 (m, 1H), 6.30-6.08 (m, 1H), 5.87-5.72 (m, 1H), 5.72-5.65 (m, 1H), 4.43-4.24 (m, 4H), 4.24-3.94 (m, 2H), 3.64-3.48 (m, 2H), 2.55 (s, 3H), 2.12-1.99 (m, 3H); MS calculated for C24H26ClN6O3 (M+H+) 481.17. found 481.2.

1. additionThe reaction was then added directly to a RediSep
2. customdry loader cartridge
3. custompurified by column chromatography (9:1:0.175 M CH2Cl2/MeOH/NH3 in CH2Cl2, 0-50%)