PEG-400为助溶剂合成(1,5-环辛二烯)氯化铑(I)二聚体

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采用PEG-400为助溶剂,研究了(1,5-环辛二烯)氯化铑二聚体制备的小试工艺条件,通过实验考察了PEG-400用量、溶剂种类、反应温度、三氯化铑浓度、配体用量等因素对产率的影响,确定了适宜的工艺条件为:2克水合三氯化铑,加12ml水,30ml无水乙醇,4ml COD,2ml PEG-400搅拌均匀,通氮气保护,油浴40℃反应5h,冷至室温,过滤,洗涤,干燥,得产品,收率在80-85%之间。 Using PEG-400 as cosolvent, the experimental conditions of preparing (1,5-cyclooctadiene) rhodium chloride dimer were studied. The effects of PEG-400 dosage, solvent type, reaction temperature, Rhodium concentration, the amount of ligand and other factors on the yield, determine the appropriate process conditions: 2 g rhodium trichloride hydrate, add 12ml water, 30ml absolute ethanol, 4ml COD, 2ml PEG-400 Stir, Nitrogen protection, oil bath 40 ℃ reaction 5h, cooled to room temperature, filtered, washed and dried to give the product yield between 80-85%.
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