13-12-2018 дата публикации
Номер: US20180354891A1
Process for manufacturing a crystalline alkali metal salt of the general formula (I) [R—CH(COO)—N(CH—COO)]M(I) wherein Mis selected from alkali metal cations, same or different, Ris selected from C-C-alkyl and CHCHCOOM, comprising the step of (b) crystallizing said alkali metal salt from an aqueous solution containing in the range of from 5 to 30% by weight of alkali metal hydroxide, referring to said aqueous solution. 1. A process for manufacturing a crystalline alkali metal salt of formula (I):{'br': None, 'sub': 1', '2', '2', '3, 'sup': '1', '[R—CH(COO)—N(CH—COO)]M\u2003\u2003(I)'}wherein{'sup': '1', 'each Mis independently an alkali metal cation, and'}{'sup': 1', '1, 'sub': 1', '4', '2', '2, 'Ris a C-C-alkyl or CHCHCOOM,'}the process comprising(b) crystallizing said alkali metal salt from an aqueous solution comprising in the range of from 5 to 30% by weight of alkali metal hydroxide, based on the weight of said aqueous solution.2. The process according to claim 1 , wherein said alkali metal salt is racemic or a mixture of enantiomers comprising predominantly the respective L-isomer with an enantiomeric excess (ee) in the range of from 0.1 to 85%.3. The process according to claim 1 , wherein Ris methyl and Mis sodium.4. The process according to claim 1 , wherein (b) comprises providing an aqueous solution of alkali metal salt of formula (I) in an aqueous solution of alkali metal hydroxide claim 1 , said solution having a temperature of at least 50° C. claim 1 , and cooling down said solution to 35° C. or less at a cooling rate of 0.1 to 1.5° C./min.5. The process according to claim 1 , wherein said crystallizing comprises cooling crystallization.6. The process according to claim 1 , further comprising (a1): [{'br': None, 'sup': 2', '2, 'sub': 2', '2, 'R—CH(COOM)-N(CH—CN)\u2003\u2003(II a)'}, {'br': None, 'sup': '2', 'sub': 2', '2, 'R—CH(CN)—N(CH—CN)\u2003\u2003(II b)'}], '(a1) saponification of at least one nitrile according to formula (II a) or (II b)'}wherein ...
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