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【答案】應(yīng)助回帖
★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ zhuzj28: 金幣+5, 翻譯EPI+1, ★有幫助 2013-04-19 13:37:09 zhuzj28: 金幣+20, ★★★★★最佳答案 2013-04-20 13:31:45
試著翻了第二段,很多專(zhuān)業(yè)的東西不是很了解:
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.
新制備出來(lái)的反應(yīng)混合物溶解在乙酸乙酯中,然后過(guò)濾,在真空條件下濃縮,最后在室溫條件下用蒸餾水水解。得到的溶液分別裝載到一列20毫升的AG-1 X8中,用一系列濃度梯度的碳酸氫三乙胺(pH=7.2,300 mL + 300 mL, 濃度為0-100毫摩爾每升)進(jìn)行溶析。含有的部分次磷酸濃縮干燥。由此得到的油狀物是與其四倍丙醇的共沸混合物,溶于水中,過(guò)一個(gè)Dowex 50 (H+)短柱子,在高真空條件下濃縮afforded the phosphinic acid
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