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zhuzj28

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huangzx1314

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【答案】应助回帖

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zhuzj28: 金币+5, 翻译EPI+1, ★有帮助 2013-04-19 13:37:09
zhuzj28: 金币+20, ★★★★★最佳答案 2013-04-20 13:31:45
试着翻了第二段,很多专业的东西不是很了解:

The crude reaction mixture was dissolved in EtOAc, filtered, concentrated in vacuo, and hydrolyzed with distilled water at rt. The resulting solution was loaded onto  a column of AG-1 X8 (20 mL) and was then eluted with a linear gradient (300 mL + 300 mL, 0-100 mM) of triethylammonium  bicarbonate (pH 7.2). Fractions containing phosphinic acid  were concentrated to dryness. The resulting oil was azeotroped  four times with 2-propanol, dissolved in water, and  passed down a short column of Dowex 50 (H+). Concentration  under high vacuum afforded the phosphinic acid.

新制备出来的反应混合物溶解在乙酸乙酯中,然后过滤,在真空条件下浓缩,最后在室温条件下用蒸馏水水解。得到的溶液分别装载到一列20毫升的AG-1 X8中,用一系列浓度梯度的碳酸氢三乙胺(pH=7.2,300 mL + 300 mL, 浓度为0-100毫摩尔每升)进行溶析。含有的部分次磷酸浓缩干燥。由此得到的油状物是与其四倍丙醇的共沸混合物,溶于水中,过一个Dowex 50 (H+)短柱子,在高真空条件下浓缩afforded the phosphinic acid

2楼2013-04-19 12:39:41
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