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CRYSTALLINE TETRAKIS(TRIPHENYLPHOSPHINE) PALLADIUM AND ITS PRODUCTION

机译:四氯化萘(三苯膦)钯及其生产

摘要

PURPOSE:To provide the subject compound useful for catalystis, etc., and capable of being industrially produced, stored and used by reacting PdCl2 with triphenyl phosphine in a polar solvent, treating the reactional product with hydrazine, filtering the crystals of the reactional product, and subsequently washing the crystals with an alcohol and with a hydrocarbon solvent. CONSTITUTION:Palladium chloride and triphenyl phosphine are added to an aprotic polar solvent (e.g. dimethyl formamide), heated up to 140 deg.C, stirred for one hour, cooled to 80 deg.C, mixed with a 25% hydrazine hydrate aqueous solution with the careful generation of nitrogen gas, stirred at 80-85 deg.C for 30min and subsequently cooled to room temperature. The produced green crystals are filtered, washed with an alcohol and further washed with a hydrocarbon solvent (e.g. n-hexane) to produce crystalline tetrakis(triphenylphosphine) palladium having a melting point of 128-131 deg.C (decomp.) and exhibiting a specific powder X-ray pattern.
机译:用途:提供主题化合物用于催化剂等,并能够通过在极性溶剂中使PdCl2与三苯基膦反应,用肼处理反应产物,过滤反应产物的晶体来工业生产,储存和使用,然后用醇和烃溶剂洗涤晶体。组成:将氯化钯和三苯基膦加入非质子极性溶剂(如二甲基甲酰胺)中,加热至140℃,搅拌1小时,冷却至80℃,与25%的水合肼水溶液混合。小心地产生氮气,在80-85℃下搅拌30分钟,然后冷却至室温。将产生的绿色晶体过滤,用醇洗涤,再用烃溶剂(例如正己烷)洗涤,以产生熔点为128-131℃(分解)的结晶四(三苯基膦)钯。特定的粉末X射线图。

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