Potassium trifluoroacetate synthesis
- Product Name:Potassium trifluoroacetate
- CAS Number:2923-16-2
- Molecular formula:C2F3KO2
- Molecular Weight:152.11
75-89-8
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$9.00/1g
2923-16-2
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$5.00/1g
Yield:2923-16-2 86%
Reaction Conditions:
Stage #1:2,2,2-trifluoroethanol with sodium hypochlorite;2,2,6,6-Tetramethyl-1-piperidinyloxy free radical;potassium bromide in acetonitrile; pH=8 - 9 at 20; for 48 h;
Stage #2: with sulfuric acid in water; pH=1 - 2
Stage #3: in methanol at 20; for 1 h;
Steps:
14
Example 14: Potassium salt of trifluoroacetic acid (CF3-COOK (5)); 20 ml water, 73 ml MeCN, 1.33 g KBr, TEMPO (0.46 g), and 10 g of trifluoroethanol are placed in a 500 ml glass flask equipped with a dropping funnel and stirrer. 175ml of 15%> wt. aq. NaOCl buffered to pH 8-9 were added via the dropping funnel in 3 portions over two days while stirring at room temperature. Concentrated sulphuric acid and water were added to make the reaction mixture acidic (pH 1 to 2). The reaction mixture was extracted three times with diethyl ether. The combined ether phases were dried over magnesium sulphate and then distilled at atmospheric pressure. Methanol (60 ml) and potassium methoxide (7 g) were added to the distillate and the mixture was stirred for one hour at room temperature, filtered and evaporated to give a colorless solid (13.13 g) Yield: 86%. 19F NMR (D20): -76.82 (s, 3F).
References:
3M INNOVATIVE PROPERTIES COMPANY;HINTZER, Klaus;VOGEL, Dennis E.;GUERRA, Miguel A.;IGNATOWSKA, Jolanta;R?SCHENTHALER, Gerd-Volker;SHYSHKOV, Oleg;VOGEL, Kim M.;ZIPPLIES, Tilman C. WO2011/50131, 2011, A2 Location in patent:Page/Page column 40
76-05-1
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$9.00/1g
2923-16-2
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$5.00/1g
353-85-5
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2923-16-2
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