Production of 3,3-dimethyl-2-oxo-butyric acid salt

Organic compounds -- part of the class 532-570 series – Organic compounds – Carboxylic acids and salts thereof

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562579, C07C 5100, C07C 51285, C07C 51373

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045647046

ABSTRACT:
Dichloropinacolone is produced by introducing into pinacolone twice the molar amount of chlorine, the exothermic reaction mass being cooled initially to maintain the temperature below about 50.degree. C. until about 60 to 80% of the chlorine has been introduced, and then heating the reaction mass to a temperature above 50.degree. C. during introducing of the remainder of the chlorine, thereby to produce dichloropinacolone, and terminating chlorine introduction when the dichloropinacolone content of the reaction mass is at least about 97%. The molten product is added to an aqueous solution of an alkali maintained at a temperature of at least about 50.degree. C., the alkali being present in more than three times the molar amount of the dichloropinacolone. To the resulting solution of a salt of 3,3-dimethyl-2-hydroxy-butyric acid, brought to a pH of about 9 to 12, there is added approximately the stoichiometric amount of potassium permanganate. Solid MnO.sub.2 precipitates out and is separated from the substantially pure dissolved salt of 3,3-dimethyl-2-oxo-butyric acid. The product is a known compound suited for further syntheses.

REFERENCES:
patent: 4052460 (1977-10-01), Dickore et al.
patent: 4113767 (1978-09-01), Merz
Wittorf, N., Chemisches Central-Blatt (1900), p. 29 of vol. II.
Beilstein, F. et al., Berichte der Deutschen Chemischen Gesellschaft, (1884), vol. 17, pp. 840-842.
Beilsteins Handbuch der Organischen Chemie, 4th Ed., (1921), vol. 3, pp. 273; 341; 608 and 697.
Dean, John A. Ed., "Lange's Handbook of Chemistry" 12th Ed., (1979), McGraw-Hill, Publ., pp. 4-75.

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