http://rdf.ncbi.nlm.nih.gov/pubchem/patent/DK-3066071-T3

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filingDate 2014-11-04-04:00^^<http://www.w3.org/2001/XMLSchema#date>
grantDate 2018-07-30-04:00^^<http://www.w3.org/2001/XMLSchema#date>
inventor http://rdf.ncbi.nlm.nih.gov/pubchem/patentinventor/MD5_ad1726b310bdcf96a81a95823b618796
http://rdf.ncbi.nlm.nih.gov/pubchem/patentinventor/MD5_bd1b0b6b5487a9c3b488b3afad748a0b
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publicationDate 2018-07-30-04:00^^<http://www.w3.org/2001/XMLSchema#date>
publicationNumber DK-3066071-T3
titleOfInvention METHOD OF PREPARING IOPAMIDOL
abstract The present invention discloses a process for the preparation of lopamidol of formula (II)n nand comprising the following steps:na) reacting the Compound (I) wherein X is OR 2 or R 3 , and wherein R 2 and R 3 are a C 1 -C 6 linear or branched alkyl, C 3 -C 6 cycloalkyl, C 6 aryl, optionally substituted with a group selected from the group consisting of methyl, ethyl, n-propyl, i-propyl, n-butyl, sec-butyl, t-butyl and phenyl, with the acylating agent (S)-2-(acetyloxy)propanoyl chloride in a reaction medium to provide the acetyloxy derivative of Compound (I);nb) hydrolyzing the intermediate from step a) with an aqueous solution at a pH comprised from 0 to 7, by adding water or a diluted alkaline solution such as sodium hydroxide or potassium hydroxide, freeing the hydroxyls from the boron-containing protective groups, obtaining the N-(S)-2-(acetyloxy)propanoyl derivative of Compound (II);nc) alkaline hydrolysis to restore the (S)-2-(hydroxy)propanoyl group and to obtain lopamidol (II) and optional recovery of the boron derivative from the solution obtained in step b).nThe boron-containing protective group is versatile, efficient and recyclable. A one-pot synthesis, without intermediate isolation is provided, leading to a decreasing of recovered and recycled solvents and a significant increasing in the yield, representing a significant advantage in terms of cost-effectiveness of the entire process and environmental awareness.
priorityDate 2013-11-05-04:00^^<http://www.w3.org/2001/XMLSchema#date>
type http://data.epo.org/linked-data/def/patent/Publication

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