US 12,129,563 B2
Electrochemical iodination of N,N′-(2,3-dihydroxypropyl)-5-hydroxy-1,3-benzenedicarboxamide
Luciano Lattuada, Cassina de' Pecchi (IT); Camilla Cavallotti, Novara (IT); Giovanni Battista Giovenzana, Novara (IT); Fulvio Uggeri, Codogno (IT); Alessandro Minguzzi, Milan (IT); Alberto Vertova, Treviglio (IT); Letizia Sorti, Dalmine (IT); and Carlo Morelli, Cambiago (IT)
Assigned to BRACCO IMAGING S.P.A., Milan (IT)
Appl. No. 18/694,306
Filed by BRACCO IMAGING S.P.A., Milan (IT)
PCT Filed Sep. 22, 2022, PCT No. PCT/EP2022/076320
§ 371(c)(1), (2) Date Mar. 21, 2024,
PCT Pub. No. WO2023/046815, PCT Pub. Date Mar. 30, 2023.
Claims priority of application No. 21198848 (EP), filed on Sep. 24, 2021; and application No. 22184631 (EP), filed on Jul. 13, 2022.
Prior Publication US 2024/0271295 A1, Aug. 15, 2024
Int. Cl. C25B 3/27 (2021.01); C07C 231/12 (2006.01); C07C 237/46 (2006.01); C25B 3/07 (2021.01); C25B 3/09 (2021.01); C25B 3/11 (2021.01); C25B 15/08 (2006.01)
CPC C25B 3/27 (2021.01) [C07C 231/12 (2013.01); C07C 237/46 (2013.01); C25B 3/07 (2021.01); C25B 3/09 (2021.01); C25B 3/11 (2021.01); C25B 15/081 (2021.01); C25B 15/083 (2021.01); C25B 15/087 (2021.01)] 15 Claims
OG exemplary drawing
 
1. A process for the preparation of N,N′-bis-(2,3-dihydroxypropyl)-5-hydroxy-2,4,6-triiodo-1,3-benzenedicarboxamide (I), comprising the steps of:
a) dissolving N,N′-(2,3-dihydroxypropyl)-5-hydroxy-1,3-benzenedicarboxamide (II) in a reaction medium in the presence of molecular iodine (I2) and
b) iodinating said compound (II) with the molecular iodine (I2) to obtain said compound (I), wherein the reaction medium is an aqueous solution and the molecular iodine (I2) is in situ electrochemically generated from a source of iodide ions (I−) and wherein steps a) and b) are carried out in
galvanostatic mode using an undivided electrolytic cell or
in potentiostatic mode using an electrolytic cell formed by two-compartments divided by a porous septum or by a ionic exchange membrane.