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Process for the preparation of a 5,5'-bi-1H-tetrazole salt

机译:制备5,5'-bi-1H-四唑盐的方法

摘要

A process for the preparation of a 5,5'-bi-1H-tetrazole diammonium salt by dropwisely adding the aqueous hydrogen peroxide to which a small amount of weakly acidic substance has been added, to a starting aqueous solution containing hydrogen cyanide or sodium cyanide or potassium cyanide, sodium azide and a catalytic amount of copper sulfate preferably at a low temperature to maintain the pH of the reaction solution over a range of from 5 to 6, heating the reaction solution to effect the oxidation and cyclization reaction, reacting the reaction product with ammonium chloride or an aqueous solution thereof, and recovering the formed ammonium salt in the form of sparingly soluble crystals. The desired product is obtained in a high yield and in a high purity from the starting materials which are cheaply available and are easy to handle through a decreased number of steps, i.e., through a one-pot reaction without requiring cumbersome after-treatment.
机译:通过将已添加了少量弱酸性物质的过氧化氢水溶液滴加到含有氰化氢或氰化钠的起始水溶液中的5,5'-bi-1H-四唑二铵盐的制备方法优选在低温下将氰化钾或氰化钾,叠氮化钠和催化量的硫酸铜保持在低温下以将反应溶液的pH维持在5至6的范围内,加热反应溶液以进行氧化和环化反应,使反应用氯化铵或其水溶液制得产物,并以微溶的晶体形式回收形成的铵盐。从廉价的起始原料以高收率和高纯度获得期望的产物,所述起始原料廉价且易于通过减少的步骤数来处理,即通过一锅法反应而无需繁琐的后处理。

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