C - Chemistry – Metallurgy – 07 – H
Patent
C - Chemistry, Metallurgy
07
H
C07H 19/10 (2006.01) C07F 9/09 (2006.01) C07H 19/20 (2006.01)
Patent
CA 2181474
The process is characterized in that a phosphoric acid ester is condensed with a compound containing hydroxy groups in the presence of an arylsulfonic acid chloride and an organic base, the residue of evaporation is stirred out with an organic solvent after the hydrolysis, the arylsulfonic acid pyridine salt which forms is nearly completely crystallized and recycled, the lipid derivative that is formed is precipitated as a sparingly soluble salt by addition of a solution containing alkaline-earth ions and isolated, the sparingly soluble salt is isolated as the free acid in an organic solvent by suspension in a water-immiscible organic solvent and a dilute aqueous mineral acid, the crude product is purified if desired, by means of preparative chromatography on a RP phase and subsequently the free acid is converted if desired into any desired salt.
L'invention a pour objet un procédé de fabrication de diesters d'acide phosphorique asymétriques. Ledit procédé est caractérisé par les étapes suivantes: condensation d'un ester d'acide phosphorique avec un composé renfermant des groupes hydroxyle en présence d'un chlorure d'arylacide sulfonique et d'une base organique; précipitation après hydrolyse du résidu d'évaporation avec un solvant organique, cristallisation quasi complète et recyclage, après hydrolyse, du sel de pyridine d'arylacide sulfonique, précipitation et isolation sous forme de sel difficilement soluble par addition d'une solution renfermant des ions alcalino-terreux, isolation du sel difficilement soluble par suspension dans un solvant organique non miscible à l'eau et dans un acide minéral, sous forme d'acide libre dans le solvant organique; le cas échéant purification du produit de base par chromatographie préparative en phase inverse puis transformation le cas échéant de l'acide libre en un sel quelconque.
Kiegel Einhard
Zilch Harald
Boehringer Mannheim Gmbh
Heidelberg Pharma Holding Gmbh
Norton Rose Or S.e.n.c.r.l. S.r.l./llp
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