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ChemicalBook CAS DataBase List Methanesulfinic acid, 1,1,1-trifluoro-

Methanesulfinic acid, 1,1,1-trifluoro- synthesis

11synthesis methods
41804-89-1 Synthesis
potassium trifluoromethanesulfonate

41804-89-1
28 suppliers
$110.00/1g

Methanesulfinic acid, 1,1,1-trifluoro-

34642-42-7
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Yield:-

Reaction Conditions:

with sulfuric acid in ethylbenzene at 20 - 30;Product distribution / selectivity;

Steps:

1
EXAMPLE 1 Azeotropic Distillation of Trifluoromethanesulfinic Acid with Ethylbenzene In a 750 ml reactor with stirrer and distillation attachment, 92.7 g of potassium trifluoromethanesulfinate (0.50 mol, 92.5%) were suspended in 142 g of ethylbenzene. Subsequently, 75.0 g of concentrated sulfuric acid (0.75 mol, 98%) were added dropwise at from 20 to 30° C. with cooling within 15 min. The trifluoromethanesulfinic acid released thereby was azeotropically distilled off under a reduced pressure of 40 mbar at a condensate temperature of 46° C. within 5 h. The 69.4 g of lower phase of the distillate cooled to 5° C. consisted of trifluoromethanesulfinic acid and small amounts of ethylbenzene. The upper phase, which consisted predominantly of ethylbenzene, ran back into the reactor continuously during the distillation. The trifluoromethanesulfinic acid thus obtained (95% yield, 92% purity) can be used in subsequent reactions without further workup.

References:

BASF SE US2011/190510, 2011, A1 Location in patent:Page/Page column 3