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xie0311

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[求助] 高分求翻译

Sodium carbonate (15.0 mg, 0.142 mmol, 1.1 equiv) was added to a suspension of digoxin (99.8 mg, 0.128 mmol, 1.0 equiv) and salicylaldehyde (77.81 μL, 0.639 mmol, 5.0 equiv) in methanol (5.1 mL, 25 mM), at which point the contents turned yellow in color. A reflux condenser was affixed to the flask and the contents were warmed to reflux in a 125 °C oil bath. The reaction was cooled to room temperature after 23 h and concentrated in vacuo. The crude material was dry-loaded onto Celite and purified by flash chromatography on silica gel (1:0 → 19:1 ethyl acetate/methanol) to afford Dig(sal) (30.3 mg, 0.0342 mmol, 27% yield) as a pale yellow solid in ~8:1 dr. Mixed fractions containing the desired compounds were repurified by flash chromatography on silica gel (1:0 → 19:1 → 9:1 dichloromethane/methanol) to yield an additional 30.1 mg (0.0340 mmol, 27% yield) of Dig(sal) in ~3:1 dr. In some cases, different batches of Dig(sal) displayed varying toxicity with human embryonic kidney (HEK) 293t cells , presumably due to minor contamination with digoxin or a digoxin-related compound. Material obtained from the conditions described above can be further purified by preparative thin -layer chromatography, developing the plate thrice with either 9:1 dichloromethane/methanol or 19:1 ethyl acetate/methanol, to afford pure Dig(sal) that does not exhibit cytotoxicity up to 16 μM with HEK 293t cell .

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xysi

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感谢参与，应助指数 +1
mouse103: 应助指数-1, 老兄是做工艺的么，这中翻译最好不要拿出来，呵呵 2012-04-22 18:58:14

碳酸钠（15.0毫克，0.142毫摩尔，1.1当量）被暂停了地高辛（99.8毫克，1.0，0.128毫摩尔当量）和醛（77.81μL，0.639毫摩尔，5.0当量）甲醇（5.1毫升，25毫米），在这一点的内容转为黄色。被贴上回流冷凝器的烧瓶和内容进行预热在125℃油浴回流。冷却至室温反应23小时后，主要集中在真空中。粗料干装上硅藻土和闪光层析纯化硅胶（1:0→19:1乙酸乙酯/甲醇）作为一个苍白的负担挖（SAL）（30.3毫克，0.0342毫摩尔，27％的产量）～8:1博士黄色固体。含有所需化合物的混合馏分repurified闪光层析硅胶（1:0→19:1→9:1二氯甲烷/甲醇）产生一个额外的30.1毫克挖（0.0340毫摩尔，27％的产量）（SAL）～3:1博士。在某些情况下，不同批次的开掘（SAL）显示不同与人类胚胎肾（HEK）293T细胞，大概是由于轻微污染与地高辛或地高辛相关化合物的毒性。从上述条件获得的材料可以进一步纯化制备薄层色谱法，开发板或者9:1的二氯甲烷/甲醇或19:1乙酸乙酯/甲醇，买得起纯挖（SAL），不会出现三次细胞毒性高达16微米HEK 293T细胞。