DE874305C - Process for the production of ferrocalcium citrate - Google Patents

Process for the production of ferrocalcium citrate

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Publication number
DE874305C
DE874305C DEO1296A DEO0001296A DE874305C DE 874305 C DE874305 C DE 874305C DE O1296 A DEO1296 A DE O1296A DE O0001296 A DEO0001296 A DE O0001296A DE 874305 C DE874305 C DE 874305C
Authority
DE
Germany
Prior art keywords
citrate
ferrocalcium
production
water
protective gas
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired
Application number
DEO1296A
Other languages
German (de)
Inventor
Adolf Christian Jose Opfermann
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Johann G W Opfermann & Sohn
Original Assignee
Johann G W Opfermann & Sohn
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Johann G W Opfermann & Sohn filed Critical Johann G W Opfermann & Sohn
Priority to DEO1296A priority Critical patent/DE874305C/en
Application granted granted Critical
Publication of DE874305C publication Critical patent/DE874305C/en
Expired legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00—Compounds of iron
    • C01G49/009—Compounds containing, besides iron, two or more other elements, with the exception of oxygen or hydrogen
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K31/00—Medicinal preparations containing organic active ingredients
    • A61K31/28—Compounds containing heavy metals
    • A61K31/295—Iron group metal compounds
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/41—Preparation of salts of carboxylic acids
    • C07C51/418—Preparation of metal complexes containing carboxylic acid moieties

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Epidemiology (AREA)
  • Medicinal Chemistry (AREA)
  • Pharmacology & Pharmacy (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)

Description

Verfahren zur Herstellung von Ferrocalciumcitrat Zusatz zum Zusatzpatent 868 869485 Gegenstand des Patents ö57363 ist die Herstellung eines therapeutisch verwertbaren Ferrocalciumcitrats der Formel CaFe2(C6Ht;O+)2 durch Umsetzung von Citronensäure in wäßriger Lösung mit Ferrum reduetum und Calciumcarbonat oder Calciumcitrat vorzugsweise in stöchiometrischen Mengen in Anwesenheit eines Schutzgases und Abtreiben des Wassers nach erfolgter Umsetzung, vorzugsweise ebenfalls in Gegenwart eines Schutzgases.Process for the production of ferrocalcium citrate Addition to the additional patent 868 869485 The subject of the patent ö57363 is the production of a therapeutic utilizable ferrocalcium citrate of the formula CaFe2 (C6Ht; O +) 2 by reaction of Citric acid in aqueous solution with Ferrum reduetum and calcium carbonate or calcium citrate preferably in stoichiometric amounts in the presence of a protective gas and stripping of the water after the reaction, preferably also in the presence of one Protective gas.

In dem Patent 869 486 wird das Verfahren des Patents 857363 dahin abgewandelt, daß die Umsetzung mit Ferrohydroxyd oder Ferrosalzen flüchtiger Säuren, insbesondere Ferrocarbonat an Stelle von Ferrum reductum, durchgeführt wird. In patent 869,486, the procedure of patent 857363 is lost modified that the reaction with ferrohydroxide or ferrous salts of volatile acids, in particular ferrocarbonate is carried out in place of Ferrum reductum.

Es wurde weiterhin gefunden, daß durch Abänderung der stöchiometrischen Mengenverhältnisse der g]eichen Ausgangsstoffe statt des in den Vorerfindungen beschriebenen Di-Ferromonocalciumcitrats der Formel CaFe2 (C6 Hb °7)2 Mono-Ferrodicalciumcitrat der Fonnel Ca2Fe(C6HfjO7)2 hergestellt werden kann. It was also found that by changing the stoichiometric Quantities of the same starting materials instead of that described in the previous inventions Di-ferromonocalcium citrate of the formula CaFe2 (C6 Hb ° 7) 2 mono-ferrodicalcium citrate the formula Ca2Fe (C6HfjO7) 2 can be produced.

Auch dieses Ferrocalciumcitrat ist in feuchtem Zustand gegen Sauerstoff empfindlich, weshalb der Luftsauerstoff bei der Umsetzung durch Anwendung eines Schutzgases, z. B. Stickstoff, Wasserstoff oder Rohlensäure, ferngehalten werden muß. Auch in diesem Fall bieten der bei der Reaktion frei werdende Wasserstoff und die Kohlensäure einen gewissen Schutz gegen Oxydation. Es ist jedoch zweckmäßig, noch zusätz- liche Schutzgase einzuleiten und auch nach erfolgter Umsetzung so lange durch die Reaktionslösung durchzuleiten, bis das Wasser abgetrieben ist. Die wasserfreie Verbindung ist gegen Luftsauerstoff beständig. This ferrocalcium citrate is also moist against oxygen sensitive, which is why the atmospheric oxygen in the implementation by applying a Protective gas, e.g. B. nitrogen, hydrogen or crude acid can be kept away got to. In this case too, the hydrogen released during the reaction and the carbonic acid a certain protection against oxidation. However, it is useful still additional initiate protective gases and also after Implementation to pass through the reaction solution until the water is driven off is. The water-free connection is resistant to atmospheric oxygen.

Beispiele I. 2 Mol Citronensäure werden in destilliertem Wasser gelöst und, um den Sauerstoff (gelöste Luft) zu vertreiben, unter Durchleiten von Wasserstoff I. Stunde zum Sieden erhitzt. Nunmehr. wird I-g-Atom Ferrum reductum in die Lösung eingebracht und beim Nachlassen der Wasserstoffentwicklung die Strömungsgeschwindigkeit des Wasserstoffs erhöht. Examples I. 2 moles of citric acid are dissolved in distilled water and, in order to drive off the oxygen (dissolved air), by passing hydrogen through it Heated to the boil for the first hour. Now. I-g-Atom Ferrum reductum will be in the solution and when the evolution of hydrogen subsides, the flow rate of hydrogen increased.

Es scheidet sich saures Ferrocitrat ab. Durch Umsetzung mit 2 Mol Calciumcarbonat wird unter Kohlensäureentwicklung das Mono-Ferrodicalciumcitrat gebildet. Das Wasser wird durch langsames Erhitzen des Reaktionsgefäßes bis auf 2000 unter gleichzeitigem Durchleiten von Wasserstoff abdestilliert, wobei ein weißes Kristallpulver zurückbleibt.Acid ferro citrate separates out. By reacting with 2 mol Calcium carbonate becomes mono-ferrodicalcium citrate with the evolution of carbonic acid educated. The water is increased by slowly heating the reaction vessel up to 2000 distilled off with simultaneous passage of hydrogen, a white Crystal powder remains.

2. Eine Lösung von 2 Mol Citronensäure in Wasser wird nach Veftreiben der gelösten Luft durch Auskochen und Durchleiten von Stickstoff mit I Mol Ferrohydroxyd versetzt. Es bildet sich saures Ferrocitrat. Hierauf wird die Lösung mit 2 Mol Calciumcarbonat versetzt, wobei sich Mono-Ferrodicalciumcitrat unter Kohlensäureentwicklung bildet. 2. A solution of 2 moles of citric acid in water is after expulsion the dissolved air by boiling and passing nitrogen through with 1 mol of ferrohydroxide offset. Acid ferro citrate is formed. Then the solution is made with 2 moles of calcium carbonate added, whereby mono-ferrodicalcium citrate is formed with the evolution of carbonic acid.

Das Durchleiten von Stickstoff wird sowohl während beider Umsetzungen als auch bis zur völligen Entfernung des Wassers fortgesetzt. Das erhaltene trockene, weiße Produkt zeigt folgende Analysendaten: gefunden: 27,o 010 C, 2,10 01o H, io,6o 01o Fell; berechnet: 28,0°/o C, I,95 O/o H, io,85 01o Fe11.The bubbling of nitrogen will occur during both reactions and continued until the water was completely removed. The obtained dry, white product shows the following analytical data: found: 27, o 010 C, 2.10 01o H, io, 6o 01o fur; Calculated: 28.0 ° / o C, 1.95 O / o H, 10.85.0 ° Fe11.

Claims (1)

PATENTANSPRUCH: Weitere Ausbildung des Verfahrens zur Herstellung von therapeutisch verwertbarem Ferrocalciumcitrat mit Ferrum reductum, Ferrohydroxyd oder Ferrosalzen flüchtiger Säuren, insbesondere Ferrocarbonat und Calciumcarbonat oder Calciumcitrat in Anwesenheit eines Schutzgases und durch Abtreibung des Wassers, vorzugsweise ebenfalls in Gegenwart des Schutzgases, nach Patent 869486, dadurch gekennzeichnet, daß zur Herstellung von Mono-Ferrodicalciumcitrat der Formel Ca2Fe(CsH507)2 entsprechende stöchiometrische Mengen der Ausgangsstoffe angewandt werden. PATENT CLAIM: Further training of the manufacturing process of therapeutically usable ferrocalcium citrate with Ferrum reductum, ferrohydroxide or ferrous salts of volatile acids, especially ferrous carbonate and calcium carbonate or calcium citrate in the presence of a protective gas and by aborting the water, preferably also in the presence of the protective gas, according to patent 869486, thereby characterized that for the production of mono-ferrodicalcium citrate of the formula Ca2Fe (CsH507) 2 Appropriate stoichiometric amounts of the starting materials are used.
DEO1296A 1950-11-22 1950-11-22 Process for the production of ferrocalcium citrate Expired DE874305C (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
DEO1296A DE874305C (en) 1950-11-22 1950-11-22 Process for the production of ferrocalcium citrate

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DEO1296A DE874305C (en) 1950-11-22 1950-11-22 Process for the production of ferrocalcium citrate

Publications (1)

Publication Number Publication Date
DE874305C true DE874305C (en) 1953-04-23

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Family Applications (1)

Application Number Title Priority Date Filing Date
DEO1296A Expired DE874305C (en) 1950-11-22 1950-11-22 Process for the production of ferrocalcium citrate

Country Status (1)

Country Link
DE (1) DE874305C (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1016251B (en) * 1955-01-22 1957-09-26 Adolf Christian Josef Opferman Process for the preparation of monomagnesium dicalcium citrate for the treatment of pulmonary tuberculosis
DE1270540B (en) * 1959-08-10 1968-06-20 Beecham Group Ltd Process for the preparation of water-soluble complex compounds of aliphatic oxycarboxylic acids

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1016251B (en) * 1955-01-22 1957-09-26 Adolf Christian Josef Opferman Process for the preparation of monomagnesium dicalcium citrate for the treatment of pulmonary tuberculosis
DE1270540B (en) * 1959-08-10 1968-06-20 Beecham Group Ltd Process for the preparation of water-soluble complex compounds of aliphatic oxycarboxylic acids

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