Process monitoring in solid phase peptide synthesis, amino group blocking effect of impure methylene chloride

Process monitoring in solid phase peptide synthesis, amino group blocking effect of impure methylene chloride
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固相肽合成过程监测,不纯二氯甲烷的氨基封闭效果

DOI:
10.1016/0014-5793(72)80076-0
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发表时间:
1972
期刊:
影响因子:
3.5
通讯作者:
T. Christensen
T. Christensen
中科院分区:
生物学3区
文献类型:
--
作者:
K. Brunfeldt;T. Christensen

文献摘要

被引文献

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在较大肽的固相合成中遇到的主要困难是缺乏对α-氨基保护基的裂解和偶联的可靠控制。已经描述了一种方法,通过该方法原则上可以执行[1,2]。采用高氯酸溶解于冰醋酸中,通过电位滴定法对悬浮于二氯甲烷和冰醋酸混合物(l/l(v/v))中的树脂结合肽进行测定。然而,通过重复滴定丙氨酸树脂,发现滴定值降低。下面描述的实验表明,滴定值的降低是由所用二氯甲烷中存在的一种或多种杂质引起的。
A major difficulty encountered in the solid phase synthesis of larger peptides is the lack of a reliable control of cleavage of the a-amino protecting group and coupling. A method by which this in principle can be performed has been described [1, 2]. The determination is carried out by potentiometric titration with perchloric acid, dissolved in glacial acetic acid, on the resin bound peptide suspended in a mixture of methylene chloride and glacial acetic acid l/l (v/v). By repeated titrations of an alanine resin, decreasing values were, however, found. Experiments are described below in which it is shown that the decrease in the titration values are caused by one or more impurities present in the methylene chloride used.