反应详情

Compound 6b was prepared by the same procedure as reported for 6a using 4c (500 mg, 1.61 mmol), ethyl N-(2-bromoethoxy)ethanamidate48 (407 mg, 1.93 mmol), DIEA (104 mg, 0.14 mL, 0.80 mmol), and DMF (5 mL). After column chromatography (elution with 7:1:0.3 chloroform:methanol:NH4OH), a yellow glassy sticky solid was obtained: yield 209 mg (30%), MS: m/z 439 (M+H)+; 1HNMR (DMSO-d6) δ 7.89 (s, 1H, H-2), 6.85 (q, 1H, 8CH3—NH), 6.47 (bs, 2H, 6-NH2), 5.69 (d, 1H, H-1′, J1′,2′=5.0 Hz), 5.27 (d, 1H, 2′-OH, J2′-2′OH=5.5 Hz), 5.06 (d, 1H, 3′-OH, J3′-3′OH=5.0 Hz), 4.88 (ddd, 1H, H-2′, J1′,2′=5.0 Hz, J2′,3′=5.8 Hz, J2′-2′OH=5.5 Hz), 4.17 (ddd, 1H, H-3′, J2′,3′=5.8 Hz, J3′,4′=4.7 Hz, J3′-3′OH=5.0 Hz), 3.86-3.95 (m, 3H, H-4′, NO—CH2), 3.92 (q, 2H, CH2CH3), 2.88 (d, 3H, 8NH—CH3, J=4.6 Hz), 2.71-2.77 (m, 1H, 5′-CH2), 2.56-2.67 (m, 3H, 5′-CH2, N(CH3)—CH2), 2.24 (s, 3H, N—CH3), 1.83 (s, 3H, C—CH3), 1.19 (t, 3H, OCH2CH3).

1. washAfter column chromatography (elution with 7:1:0.3 chloroform:methanol:NH4OH)
2. customa yellow glassy sticky solid was obtained