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Separation of citalopram intermediate from its acetate by solvent extraction

机译：通过溶剂萃取将西酞普兰中间体与乙酸盐分离

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摘要

A new method to separate citalopram intermediate (diol), one of chiral aromatic amino-alcohols, from its acetate after lipase-catalyzed kinetic resolution using liquid-liquid extraction was developed. Diol was firstly derivatized with anhydrides and then extracted with different solvent systems. The effects of pH and initial diol acetate concentration on the total distribution coefficients of diol acetate were investigated. It was found that succinic anhydride was the best derivative agent and water/toluene was the optimal extraction system. The extraction conditions with initial diol acetate concentration of 10 mmol/L, pH 8.0 were applied to the practical extraction process of the mixture of diol and diol acetate obtained by lipase-catalyzed reaction. After three extraction stages at 25 °C, the purity of diol was 99.5% and the yield achieved 86.2%.
机译：开发了一种新的方法，该方法通过液-液萃取在脂肪酶催化的动力学拆分后从其乙酸盐中分离出手性芳香族氨基醇之一西酞普兰中间体（二醇）。首先用酸酐将二醇衍生化，然后用不同的溶剂体系萃取。研究了pH和乙酸二醇酯初始浓度对乙酸二醇酯总分配系数的影响。发现琥珀酸酐是最佳的衍生物，水/甲苯是最佳的萃取系统。以初始乙酸乙二醇酯浓度为10 mmol / L，pH 8.0的提取条件为实际条件，对脂肪酶催化反应得到的二醇与乙酸乙二醇酯的混合物进行了提取。在25°C下经过三个萃取阶段后，二醇的纯度为99.5％，收率达到86.2％。

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