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ChemicalBook CAS DataBase List Perfluorobutyl iodide
423-39-2

Perfluorobutyl iodide synthesis

12synthesis methods
Add 10 mol of triphenylphosphine chloride and 50 mol of N-methylimidazole hydrochloride to methanol and stir to dissolve. Heat to 50°C, add 65 moles of aluminum chloride, stir and dissolve, continue the reaction for 2 hours, raise the temperature to 80°C, evaporate the solvent, and filter to remove the insoluble matter to obtain quaternary ammonium salt and N-alkyl imidazole salt composite aluminum acid. Salt ionic liquid. Add 2 kg of the aluminate ionic liquid prepared in step S1 to the reaction kettle equipped with a reflux device, then add 264 g of perfluoropentanoic acid and raise the temperature to 80°C. Slowly add 2.5 mol of iodine ethanol solution dropwise within 5 hours. After the dropwise addition is completed, heat to 100°C for 8 hours. The reaction solution was allowed to stand and separated into layers to separate the aluminate ionic liquid and product layers. The product layer was purified by distillation to obtain 336g of Perfluorobutyl iodide.
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Yield:423-39-2 336 g

Reaction Conditions:

with iodine in ethanol at 80 - 100; for 13 h;Reagent/catalyst;

Steps:

1.2; 2.2; 3.2; 4.2 Preparation of S2, perfluoroiodobutane

2 kg of the aluminate ionic liquid prepared in the step S1 is added to the reaction vessel equipped with the reflux device,Then, 264 g of perfluoropentanoic acid was added, and the temperature was raised to 80 ° C, and 2.5 mol of iodine in ethanol was slowly added dropwise over 5 hours.Heating was continued to 100 ° C for 8 hours, and the reaction solution was allowed to stand for separation to separate the aluminate ionic liquid layer and the product layer.The product layer was purified by rectification to obtain 336 g of perfluoroiodobutane with a HPLC purity of 98.2%.

References:

CN109651073,2019,A Location in patent:Paragraph 0022; 0025-0027; 0032; 0035-0037; 0042; 0045; 0046

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