反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
The procedure was the same as reported above for 7a using 8c (190 mg, 0.41 mmol) and 2N H2SO4 (3 mL). The compound was purified by column chromatography (elution with 4:1:0.5 chloroform:methanol:NH4OH): yield 208 mg (82%), MS: m/z 384 (M+H)+; 1HNMR (DMSO-d6) δ 10.45 (bs, 1H, 8-OH), 8.05 (s, 1H, H-2), 6.58 (bs, 2H, 6-NH2), 5.77 (d, 1H, H-1′, J1′,2′=5.0 Hz), 5.37-5.71 (bm, 2H, O—NH2), 4.83 (t, 1H, H-2′, J2′,3′=4.2 Hz), 4.18-4.29 (m, 2H, H-3′, H-4′), 3.88 (t, 2H, NH2O—CH2), 3.34-3.54 (m, 2H, 5′-CH2), 3.06 (bt, 2H, N(CH3)—CH2), 2.73 (s, 3H, N—CH3), 1.46-1.74 (bm, 4H, NH2OCH2—CH2CH2); UV λmax, nm, pH 1, 263.3 (∈ 12,200), pH 7, 268.9 (∈ 13,600), pH 13, 279.9 (∈ 15,600). Anal. (C15H25N7O5.1.9H2SO4.0.1C2H5OH.2H2O) C, H, N, S.
WORKUP
后处理
- customThe compound was purified by column chromatography (elution with 4:1:0.5 chloroform:methanol:NH4OH)