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ChemicalBook CAS DataBase List Perfluorohexanoic acid

Perfluorohexanoic acid synthesis

14synthesis methods
-

Yield:307-24-4 75%

Reaction Conditions:

with 2,2'-azobis(2-methylpropionamidine) dihydrochloride;water at 55; for 6.5 h;

Steps:

4

Example 4: Conversion of the sulphinate [5] to the carboxylic acid 4.06 g of sulphinate [5] (0.01 mol) and 30 g of demineralized water are charged to a 250 ml three-necked round-bottomed flask equipped with a mechanical stirrer, an upright reflux condenser and a temperature probe. The mixture is heated to 55 C and then a solution of 0.34 g of 2,2'-azobis- (2-methylpropionamidine) hydrochloride (Aldrich) in 20 g of water is added thereto dropwise over 1 h 30. After stirring at 55 C for 5 hours, the gel formed is extracted with 50 g of diisopropyl ether at 30 C in the presence of 10 g of NaCl. The organic phase is washed with a saturated NaCl solution to pH 3.5 and then dried over Na2S04. After evaporating the solvent under vacuum, a light yellow liquid is collected with a yield of 75%. It exhibits, in the IR spectrum, a band characteristic of the-COOH groups in the a position with respect to a-CF2 group at 1770 cm-1. The NMR analysis shows that it is essentially carboxylic acid C5F11COOH (C2F5-(C2F4) -CF2COOH), partially in the carboxylate form.

References:

WO2005/121060,2005,A1 Location in patent:Page/Page column 6-7

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