反应详情

To a solution of 1-(2-nitro-benzenesulfonyl)-piperazin-2-one HCl salt (0.76 g, 2.36 mmol), [6-N-(benzhydryloxycarbonyl)-adenin-9-yl]-acetic acid (1.0 g, 2.47 mmol), and PyBOP (1.35 g) in DMF (20 mL) was added N,N-diisopropylethylamine (0.95 mL) at 5° C. After stirring for additional 2 h, the reaction mixture was diluted with ethyl acetate (200 mL) and water (150 mL). The organic layer was separated and washed with water, 5% aqueous sodium bicarbonate, 10% aqueous citric acid, and brine. The organic layer was dried over sodium sulfate and concentrated in reduced pressure. The residue was purified by column chromatography to give the title compound (830 mg, 58%). 1H NMR (DMSO-d6) δ 10.95 (s, 1H), 8.59 (s, 0.6H), 8.58 (s, 0.4H), 8.40˜8.36 (m, 1H), 8.33 (s, 0.6H), 8.31 (s, 0.4H), 8.14 (d, 1H), 8.06˜7.96 (m, 2H), 7.54˜7.27 (m, 10H), 6.82 (s, 1H), 5.39 (s, 1.2H), 5.30 (s, 0.8H), 4.56 (s, 0.8H), 4.27 (s, 1.2H), 4.12˜4.08 (m, 2.4H), 3.92˜3.86 (m, 1.6H).

1. customThe organic layer was separated
2. washwashed with water, 5% aqueous sodium bicarbonate, 10% aqueous citric acid, and brine
3. dry with materialThe organic layer was dried over sodium sulfate
4. concentrationconcentrated in reduced pressure
5. customThe residue was purified by column chromatography