Simplified method for the preparation of aromatic sulfuric acid esters
Simplified method for the preparation of aromatic sulfuric acid esters
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DOI：
10.1021/ja01857a508
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发表时间：
1941-07-01
影响因子：
15
通讯作者：
Neuberg, CA
中科院分区：
文献类型：
--
作者：
Feigenbaum, J;Neuberg, CA
芳香族硫酸酯存在于正常尿液中，尤其是病理性尿液中。自从发现能裂解芳香族硫酸酯的酚硫酸酯酶以来，芳香族硫酸酯的分离就变得十分重要。[1] Neuberg及其合作者[2]普遍使用和改进的方法是根据Czapek的方法。3类似于这种方法，将氯磺酸加入到冰冷的吡啶氯仿溶液中，然后加入苯酚吡啶溶液中。氯仿首先在真空中蒸馏出来。然后用浓氢氧化钾水溶液使混合物呈碱性，并通过第二次真空蒸馏除去吡啶。用热乙醇从残渣中提取得到酯钾盐，冷却后以结晶形式分离。应当指出，鉴于战争在某些国家造成的情况，很难获得纯吡啶。因此，在上述程序中，我们
The aromatic sulfuric acid esters are found in normal and especially in pathological urine. Since the discovery of pheno-sulfatase, which splits the aromatic sulfuric acid esters, the prepara-tion of the esters has become significant. 1 The pro-cedure generally used andimproved by Neuberg and collaborators2 is that according to Czapek. 3 Analogous to this method chlorosulfonic acid is added to an ice-cooled solution of pyridine in chloroform and then a solution of phenol in pyridine. The chloroform is first distilled off in vacuo. The mixture is then made alkaline with strong aqueous potassiumhydroxide and the pyri-dine is removed by a second distillation in vacuo. The ester potassiumsalt is obtained from the residue by extraction with hot alcohol, from which it separates in crystalline form upon cooling. It should be remarked that, in view of thesitua-tion caused in some countries by the war, there is great difficulty in procuring pure pyridine. We, therefore, in the above-mentioned procedure, sub-