CH342965A - Process for the purification of 5-amino-salicylic acid - Google Patents
Process for the purification of 5-amino-salicylic acidInfo
- Publication number
- CH342965A CH342965A CH342965DA CH342965A CH 342965 A CH342965 A CH 342965A CH 342965D A CH342965D A CH 342965DA CH 342965 A CH342965 A CH 342965A
- Authority
- CH
- Switzerland
- Prior art keywords
- amino
- acid
- salicylic acid
- iron
- filtered
- Prior art date
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C229/00—Compounds containing amino and carboxyl groups bound to the same carbon skeleton
- C07C229/52—Compounds containing amino and carboxyl groups bound to the same carbon skeleton having amino and carboxyl groups bound to carbon atoms of six-membered aromatic rings of the same carbon skeleton
- C07C229/54—Compounds containing amino and carboxyl groups bound to the same carbon skeleton having amino and carboxyl groups bound to carbon atoms of six-membered aromatic rings of the same carbon skeleton with amino and carboxyl groups bound to carbon atoms of the same non-condensed six-membered aromatic ring
- C07C229/64—Compounds containing amino and carboxyl groups bound to the same carbon skeleton having amino and carboxyl groups bound to carbon atoms of six-membered aromatic rings of the same carbon skeleton with amino and carboxyl groups bound to carbon atoms of the same non-condensed six-membered aromatic ring the carbon skeleton being further substituted by singly-bound oxygen atoms
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Description
Verfahren zur Reinigung von 5-Amino-salizylsäure
Die Erfindung bezieht sich auf ein Verfahren zur Reinigung von 5-Amino-salizylsäure.
5-Amino-salizylsäure oder ihre Salze sind sehr wirksame Heilmittel gegen Tuberkulose sowie gegen Rheumatismus. Käufliche technische 5-Amino-salizylsäure, welche ein Zwischenprodukt der Teerfarbenfabrikation darstellt, muss sorgfältig gereinigt werden, bevor sie zu den Heilzwecken benutzt wird.
Die Reinigung ist nicht einfach, weil 5-Aminosalizylsäure sich sehr leicht oxydiert. Wenn man die Reinigung in Gegenwart von Reduktionsmitteln, z. B. von Sulfiten, durchführt und zur Entfärbung von Eisenionen befreite Aktivkohle verwendet, dann erhält man ein ganz farbloses Produkt. Die Eisenionen wirken katalytisch auf den Oxydationsprozess der 5-Amino-salizylsäure, wie man festgestellt hat.
Das Verfahren zur Reinigung von 5-Aminosalizylsäure gemäss der vorliegenden Erfindung ist dadurch gekennzeichnet, dass man die 5-Aminosalizylsäure mittels Salzsäure in Gegenwart von Natriumsulfit in das Chlorhydrat überführt, mit eisenfreier Aktivkohle entfärbt, aussalzt, abfiltriert, nach Auflösen noch einmal entfärbt und die Säure mittels Natronlauge, welche Natriumsulfit enthält, ausfällt.
Beispielsweise wird die 5-Amino-salizylsäure mittels Salzsäure, welche ein wenig Natriumsulfit enthält, in ihr Chlorhydrat übergeführt, dann entfärbt man die saure Lösung mittels eisenfreier Aktivkohle, salzt aus und filtriert ab. Nach der Auflösung des Chlorhydrats in Wasser und einer zweiten Entfärbung fällt man die 5-Amino-salizylsäure mit Natronlauge, welche ein wenig Natriumsulfit enthält, aus. Nach Anfiltrieren, Auswaschen und Trocknen erhält man ein schneeweisses Produkt, welches genügend rein ist zu Heilzwecken.
Beispiel
500 g 31 0/o technische 5-Amino-salizylsäure löst man in 1 Liter Wasser unter Zusatz von 130 g Salzsäure, gibt 20 g eisenfreie Aktivkohle und 2 g Na2SO3 zu und filtriert. Dann wird das Chlorhydrat ausgesalzt, abfiltriert und mit Salzwasser gewaschen.
Das Chlorhydrat löst man in 1 Liter Wasser, gibt 20 g gereinigte, eisenfreie Aktivkohle zu. Nach dem Abfiltrieren fällt man die 5-Amino-salizylsäure mit einer Lösung von 40 g NaOH und 2 g Na2SO3 in 400 g Wasser aus. Die Säure wird abfiltriert, gewaschen und getrocknet.
PATENTANSPRUCH
Verfahren zur Reinigung von 5-Amino-salizylsäure, dadurch gekennzeichnet, dass man die 5-Aminosalizylsäure mittels Salzsäure in Gegenwart von Natriumsulfit in das Chlorhydrat überführt, mit eisenfreier Aktivkohle entfärbt, aussalzt, abfiltriert, nach Auflösen noch einmal entfärbt und die Säure mittels Natronlauge, welche Natriumsulfit enthält, ausfällt.
**WARNUNG** Ende DESC Feld konnte Anfang CLMS uberlappen**.
Process for the purification of 5-amino-salicylic acid
The invention relates to a process for the purification of 5-amino-salicylic acid.
5-Amino-salicylic acid or its salts are very effective remedies for tuberculosis as well as for rheumatism. Commercially available technical 5-amino-salicylic acid, which is an intermediate product in the manufacture of tar paint, must be carefully cleaned before it is used for medicinal purposes.
It is not easy to clean because 5-aminosalicylic acid oxidizes very easily. When cleaning in the presence of reducing agents, e.g. B. of sulfites, and using activated carbon freed from iron ions to decolorize, then a completely colorless product is obtained. The iron ions have a catalytic effect on the oxidation process of 5-amino-salicylic acid, as has been established.
The process for the purification of 5-aminosalicylic acid according to the present invention is characterized in that the 5-aminosalicylic acid is converted into the chlorohydrate by means of hydrochloric acid in the presence of sodium sulfite, decolorized with iron-free activated carbon, salted out, filtered off, after dissolving again decolorized and the acid by means of sodium hydroxide solution, which contains sodium sulfite, precipitates.
For example, the 5-amino-salicylic acid is converted into its chlorohydrate using hydrochloric acid, which contains a little sodium sulfite, then the acidic solution is decolorized using iron-free activated carbon, salted out and filtered off. After the chlorohydrate has dissolved in water and a second decolorization, the 5-amino-salicylic acid is precipitated with sodium hydroxide solution, which contains a little sodium sulfite. After filtering, washing out and drying, a snow-white product is obtained which is sufficiently pure for medicinal purposes.
example
500 g of 31% technical-grade 5-amino-salicylic acid are dissolved in 1 liter of water with the addition of 130 g of hydrochloric acid, 20 g of iron-free activated carbon and 2 g of Na2SO3 are added and the mixture is filtered. Then the chlorohydrate is salted out, filtered off and washed with salt water.
The chlorine hydrate is dissolved in 1 liter of water and 20 g of purified, iron-free activated carbon is added. After filtering off, the 5-amino-salicylic acid is precipitated with a solution of 40 g of NaOH and 2 g of Na2SO3 in 400 g of water. The acid is filtered off, washed and dried.
PATENT CLAIM
Process for the purification of 5-amino-salicylic acid, characterized in that the 5-aminosalicylic acid is converted into the hydrochloric acid by means of hydrochloric acid in the presence of sodium sulfite, decolorized with iron-free activated carbon, salted out, filtered off, after dissolving again decolorized and the acid by means of sodium hydroxide solution, which contains sodium sulfite, precipitates.
** WARNING ** End of DESC field could overlap beginning of CLMS **.
Claims (1)
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
PL342965X | 1955-03-31 |
Publications (1)
Publication Number | Publication Date |
---|---|
CH342965A true CH342965A (en) | 1959-12-15 |
Family
ID=19936257
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CH342965D CH342965A (en) | 1955-03-31 | 1956-03-28 | Process for the purification of 5-amino-salicylic acid |
Country Status (1)
Country | Link |
---|---|
CH (1) | CH342965A (en) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO1981002671A1 (en) * | 1980-03-20 | 1981-10-01 | Ferring Farma Lab | Pharmaceutical composition and method for the treatment of colitis ulcerosa and crohn's disease by oral administration |
EP0291159A2 (en) * | 1987-04-01 | 1988-11-17 | Dak-Laboratoriet A/S | Aminosalicylic-acid derivatives for the treatment of psoriasis |
-
1956
- 1956-03-28 CH CH342965D patent/CH342965A/en unknown
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO1981002671A1 (en) * | 1980-03-20 | 1981-10-01 | Ferring Farma Lab | Pharmaceutical composition and method for the treatment of colitis ulcerosa and crohn's disease by oral administration |
EP0291159A2 (en) * | 1987-04-01 | 1988-11-17 | Dak-Laboratoriet A/S | Aminosalicylic-acid derivatives for the treatment of psoriasis |
US4933330A (en) * | 1987-04-01 | 1990-06-12 | Dak-Laboratoriet | Benzoic acid derivatives and use thereof |
EP0291159A3 (en) * | 1987-04-01 | 1993-03-17 | Dak-Laboratoriet A/S | Aminosalicylic-acid derivatives for the treatment of psoriasis |
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