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        Tetrabutylammonium hexafluorophosphate
        
    

    

        

            

                3109-63-5
            

        

        

            Tetrabutylammonium hexafluorophosphate synthesis
        

        
4synthesis methods

        
    


    
    

        
        

            
            
            
            

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Yield:3109-63-5 88%  

                
                
Reaction Conditions:

                
 with potassium hexafluorophosphate in dichloromethane;water at 20; for 24 h;

                
                
Steps:

                

                    1 Preparation Description (1): Synthesis of [(n-Bu4)N] [PF6]
K[PF6] (2.055 g, 11.2 mmol) was dissolved in 30 ml of H20. [(n-Bu4)N]Br (3.601 g, 11.2 mmol) was dissolved in 30 ml of CH2C12 and added to the aqueous solution of K[PF6]. After stirring for 24 hours at ambient temperature the phases were separated. The organic phase was washed three times with 10 ml of water dried over anhydrous Na2C03 and filtered. The filtrate was concentrated on a rotary evaporator to obtain a white solid. The obtained solid was dried at 80°C in vacuum for 18 hours. The yield of [(n-Bu4)N][PF6] was 3.822 g (88 %, 9.87 mmol).DSC (10 K/min): m.p. = 250°C, Tdec = 388°C C/H/N Analysis calc. % (found): C 49.60 (49.97), H 9.37 (9.00), N 3.61 (3.61) 1H NMR (25°C, CD3CN, 300.13 MHz, delta in ppm): 0.96 (t, 12H, CH3), 1.34 (m, 8H, CH3-CH2), 1.59 (m, 8H, CH2-CH2N), 3.06 (m, 8H, NCH2) 19F NMR (25°C, CD3CN, 300.13 MHz, delta in ppm): -73.0 (d, 6F, PF6, ^P-^F) = 706.7 Hz) 31P NMR (25°C, CD3CN, 300.13 MHz, delta in ppm): -144.6 (sept, IP, PF6, ^P-^F) = 706.7 Hz) IR (ATR, 32 scans, v in cm"1): 2966 (m), 2937 (w), 2879 (w), 1472 (m), 1404 (w), 1386 (w), 1360 (w), 1350 (w), 1319 (w), 1260 (w), 1242 (w), 1165 (w), 1109 (w), 1070 (w), 1035 (w), 931 (w), 880 (m), 829 (s), 738 (m), 555 (s)
                

                
                
References:

                

                    LONZA LTD;SIEVERT, Katharina;SCHULZ, Axel;HARLOFF, J?rg;STOFFERS, Alrik;ELLINGER, Stefan;OTT, Lothar;RIJKSEN, Christiaan;FRANKE, Patrick;TAESCHLER, Christoph;ZUR TAESCHLER, Cornelia WO2014/167034, 2014, A2  Location in patent:Page/Page column 48; 49
                

                
                
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