# US 5,703,245 A · Process for reducing water and polar impurities in imido-alkanpercarboxylic acids > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 5,703,245 A - Document ID: US5703245A - Status: Granted - Kind: A - Application number: 08/777,697 - Filed: 1996-12-20 - Granted: 1997-12-30 - Earliest claimed: 1995-12-21 - Assignees: Ausimont S.p.A. - Inventors: Claudio Cavallotti; Gilberto Nucida; Claudio Troglia - Web page: https://patentgrep.com/patent/US5703245A ## CPC - C07D 209/48: with oxygen atoms in positions 1 and 3, e.g. phthalimide - C07D: HETEROCYCLIC COMPOUNDS (macromolecular compounds C08) ## Abstract Process for reducing the content of water in imido-alkanpercarboxylic acids comprising heating a suspension of imido-alkanpercarboxylc acid in water up to the complete solid melting and subsequent separation of the organic phase from the aqueous phase and recovery of the organic phase containing the imido-alkanpercarboxylic acid. ## Claims ### Claim 1 Process for reducing the content of water in imido-alkanpercarboxylic acids having a content in water higher than 12% by weight, which comprises heating a suspension of imido-alkanpercarboxylc acid in water up to the complete solid melting and subsequent separation of an organic phase from an aqueous phase and recovery of the organic phase containing the imido-alkanpercarboxylic acid. ### Claim 2 (depends on 1) Process for reducing the content of water in imido-alkanpercarboxylic acids according to claim 1, wherein the imido-alkanpercarboxylic acids have the general formula: ##STR6## wherein A indicates a group of formula ##STR7## n is an integer 0, 1 or 2, R.sup.1 is hydrogen, chlorine, bromine, alkyl C.sub.1 -C.sub.20, alkenyl C.sub.2 -C.sub.20, aryl or alkylaryl, R.sup.2 is hydrogen, chlorine, bromine or a group of formula --SO.sub.3 M, --CO.sub.2 M, --CO.sub.3 M, --OSO.sub.3 M, M indicates hydrogen, an alkaline metal or ammonium ion or the equivalent of an alkaline-earth metal ion and X indicates alkylene C.sub.1 -C.sub.19 or arylene; Y is .dbd.X. ### Claim 3 (depends on 2) Process for reducing the content of water in imido-alkanepercarboxylic acids according to claim 2, wherein Y is an alkylene C.sub.3 -C.sub.19. ### Claim 4 (depends on 1) Process for reducing the content of water in imido-alkanpercarboxylic acids according to claim 1, wherein the acid is the phthalimido-peroxyhexanoic acid. ### Claim 5 (depends on 4) Process for reducing the content of water in imido-alkanpercarboxylic acids according to claim 4, wherein the acid is phthalimido-peroxyhexanoic acid and the melting temperature of the eutectic is about 72.degree. C. ### Claim 6 (depends on 1) Process for reducing the content of water in imido-alkanpercarboxylic acids according to claim 1, wherein the imido-alkanpercarboxylic acids are obtainable by peroxidation processes in the presence of hydrogen peroxide and of a strong acid of an imido-alkancarboxylic acid precursor obtainable by reaction of A) a1) an anhydride of formula ##STR8## or the corresponding acids, with b1) an aminoacid of formula ##STR9## with c1) water; or a1) with b2) a lactam of general formula ##STR10## with c1) water; at temperatures comprised betweeen 100.degree. C. and 250.degree. C., under pressure of an inert gas from 1 to 30 bar, for reaction times from 2 to 20 hours; the meaning of the symbols being the one indicated above. ### Claim 7 (depends on 6) Process for reducing the content of water in imido-alkanpercarboxylic acids according to claim 6, wherein the imido-alkanpercarboxylic acids are phthalimido-peracetic acid, 3-phthalimido-perpropionic acid, 4-phthalimido-perbutyric acid, 2-phthalimido-diperglutaric acid, 2-phthalimido-dipersuccinic acid, 3-phthalimido-perbutyric acid, 2-phthalimido-perpropionic acid, 3-phthalimido-diperadipic acid, naphthalimido-peracetic acid, 2-phthalimido-monopersuccinic acid. ### Claim 8 (depends on 6) Process for reducing the content of water in imido-alkanpercarboxylic acids according to claim 6, wherein the peroxidation reaction is carried out in solvent. ### Claim 9 (depends on 8) Process for reducing the content of water in imido-alkanpercarboxylic acids according to claim 8, wherein the solvent is chosen between CH.sub.2 Cl.sub.2 and CHCl.sub.3. ### Claim 10 (depends on 1) Process for reducing the content of water in imido-alkanpercarboxylic acids according to claim 1, wherein sequestering agents are added. ### Claim 11 (depends on 10) Process for reducing the content of water in imido-alkanpercarboxylic acids according to claim 10, wherein the sequestering agents are selected from hydroxycarboxylic acids, amino-polycarboxylic acids, pyridin-carboxylic acids, polyphosphonic acids. ### Claim 12 (depends on 1) Process for reducing the content of water in imido-alkanpercarboxylic acids according to claim 1, wherein the organic phase of the melt is solidified on a cooled belt. ### Claim 13 (depends on 1) Process for reducing the content of water in imido-alkanpercarboxylic acids according to claim 1, wherein the melted organic phase is submitted to a stripping treatment with reduced pressure vapour. ### Claim 14 (depends on 13) Process for reducing the content of water in imido-alkanpercarboxylic acids according to claim 13, wherein the vapour is passed in counter-current. ### Claim 15 (depends on 1) Process for the purification of imido-alkanpercarboxylic acids from polar impurities according to claim 1, comprising heating of a suspension of imido-alkanpercarboxylic acid in water up to the complete melting of the solid, and subsequent separation of the organic phase from the aqueous phase and recovery of the organic phase containing the imido-alkanpercarboxylic acid. ### Claim 16 Process for the purification of imido-alkanpercarboxylic acids from polar impurities comprising heating of a suspension of imido-alkanpercarboxylic acid in water up to the complete melting of the solid, and subsequent separation of an organic phase from an aqueous phase and recovery of the organic phase containing the imido-alkanpercarboxylic acid. ### Claim 17 (depends on 16) Process for the purification of imido-alkanpercarboxylic acids from polar impurities according to claim 16, wherein the organic phase of the melt is solidified in a mass of cool water.