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lgq101木虫 (小有名气)
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[求助]
求翻译实验过程~~~谢谢
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| General Procedure for Monitoring Solid-Phase Reactions. An aliquot of vacuum-dried resin (4 mg) was swollen with THF (5 mL) for 10 min. A solution of 4-methoxybenzylalcohol (internal standard) (25 mM in THF, 1 eq) was added, followed by tetra-n-butylammonium fluoride (0.1 M in THF, 3 eq). After stirring for 2 h, the THF solution was recovered from the resin, and the solution concentrated by rotary evaporation. The residue was taken up in CH3CN (300 μL) and filtered through a Pasteur pipette with a 0.5-inch plug of normal phase silica gel over a 0.5-inch plug of reverse-phase silica gel. The plug was rinsed carefully with 3 mL CH3CN, and the crude cleavage products were recovered by rotary evaporation. HPLC analysis (ELSD) was used to determine the ratio of cleaved scaffold to internal standard, and the yield was calculated based on a calibration curve. Analysis by 1H-NMR was used to determine product ratios where appropriate. |
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zuodg
铁杆木虫 (正式写手)
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【答案】应助回帖
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ringzhu(金币+1): O(∩_∩)O~ 2011-06-04 13:12:28
lgq101(金币+10, 翻译EPI+1): 谢谢~~~~ 2011-06-04 15:43:01
ringzhu(金币+1): O(∩_∩)O~ 2011-06-04 13:12:28
lgq101(金币+10, 翻译EPI+1): 谢谢~~~~ 2011-06-04 15:43:01
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固相合成一般流程 大孔树脂4mg真空干燥，5ml THF消化10min。4-甲氧基苯甲醇溶液用作内参（25mM, THF溶解）,随后加入4-正丁基氟化铵（0.1M,THF溶解）。搅拌2h，除去大孔树脂中的THF溶液，悬蒸法浓缩THF溶液。300 ul乙腈溶解残留物，取0.5 英寸正相硅胶插头置于0.5英寸反向硅胶插头之上，巴氏吸管过滤。插头用3ml乙腈仔细清洗，初级裂解产物使用悬蒸回收。HPLC法测定裂解比例，根据平衡曲线计算得率。分析1H谱数据，评估适当条件下的产物得率。 很多专业东西不懂，楼主多指教 |
2楼2011-06-04 13:06:03