反应详情

The procedure was the same as reported above for 4a using 3b (1.00 g, 3.18 mmol) and 33% methylamine/ethanol solution (30 mL). After column chromatography (elution with 5:1:0.3 chloroform:methanol:NH4OH), a yellow glassy solid was obtained: 498 mg (50%); MS m/z 309 (M+H)+; 1HNMR (DMSO-d6) δ 8.08 (bs, 1H, H-2), 7.13 (bs, 2H, 6-NH2), 5.70 (d, 1H, H-1′, J1′,2′=6.6 Hz), 5.30 (d, 1H, 2′-OH, J2′-2′OH=6.4 Hz), 5.16 (d, 1H, 3′-OH, J3′-3′OH=4.5 Hz), 5.08 (ddd, 1H, H-2′, J1′,2′=6.6 Hz, J2′,3′=5.4 Hz, J2′-2′OH=6.4 Hz), 4.14-4.18 (m, 1H, H-3′), 3.96-4.0 (m, 1H, H-4′), 2.88 (q, 2H, 8-CH2CH3), 2.64-2.78 (m, 2H, 5′-CH2), 2.29 (s, 3H, 5′NH—CH3), 1.30 (t, 3H, 8CH2CH3).

1. washAfter column chromatography (elution with 5:1:0.3 chloroform:methanol:NH4OH)
2. customa yellow glassy solid was obtained