DE600400C - Process for the production of growth hormones or their esters - Google Patents

Process for the production of growth hormones or their esters

Info

Publication number
DE600400C
DE600400C DEI47327D DEI0047327D DE600400C DE 600400 C DE600400 C DE 600400C DE I47327 D DEI47327 D DE I47327D DE I0047327 D DEI0047327 D DE I0047327D DE 600400 C DE600400 C DE 600400C
Authority
DE
Germany
Prior art keywords
production
growth hormones
esters
solution
main patent
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
DEI47327D
Other languages
German (de)
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.)
IG Farbenindustrie AG
Original Assignee
IG Farbenindustrie AG
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 IG Farbenindustrie AG filed Critical IG Farbenindustrie AG
Priority to DEI47327D priority Critical patent/DE600400C/en
Application granted granted Critical
Publication of DE600400C publication Critical patent/DE600400C/en
Expired legal-status Critical Current

Links

Classifications

    • 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
    • A61K31/33—Heterocyclic compounds
    • A61K31/395—Heterocyclic compounds having nitrogen as a ring hetero atom, e.g. guanethidine or rifamycins
    • A61K31/435—Heterocyclic compounds having nitrogen as a ring hetero atom, e.g. guanethidine or rifamycins having six-membered rings with one nitrogen as the only ring hetero atom
    • A61K31/44—Non condensed pyridines; Hydrogenated derivatives thereof

Description

Verfahren zur Gewinnung von Wuchshormonen bzw. deren Estern Durch das Patent 586 2¢6 wird ein Verfahren zur Gewinnung von Wuchshormonen bzw. ihren Estern geschützt. Dieses Verfahren besteht im wesentlichen darin, daß man die pflanzliche Wuchshormone enthaltenden Ausgangsstoffe aus saurer Lösung in einer mit Wasser nicht mischbaren organischen Flüssigkeit aufnimmt, aus der erhaltenen Lösung die Wuchsstoffe durch Alkalien extrahiert und gegebenenfalls aus der alkalischen Lösung die Wirkstoffe durch Ansäuern abscheidet und weiter reinigt. Die alkalilöslichen Wirkstoffe können in ebenfalls wirksame neutrale Produkte durch Behandlung mit Säuren umgewandelt werden.Process for the production of growth hormones or their esters the patent 586 2 ¢ 6 is a process for the production of growth hormones or their Esters protected. This procedure consists essentially in the fact that one the vegetable Starting materials containing growth hormones from acidic solution in one with water do not absorbs miscible organic liquid, the growth substances from the solution obtained extracted by alkalis and optionally the active ingredients from the alkaline solution separated by acidification and further purified. The alkali-soluble active ingredients can converted into equally effective neutral products by treatment with acids will.

Bei der weiteren Bearbeitung des Gegenstandes der Erfindung des Hauptpatents hat sich nun gezeigt, daß gekeimte Samen, z. B. gute Malzsorten, ein besonders ergiebiges Ausgangsmaterial für die Gewinnung der Wuchshormone sind, und daß man diese Wirkstoffe daraus in guter Ausbeute erhalten kann, wenn man die im Hauptpatent angegebenen Arbeitsweisen auf dieses Ausgangsmaterial anwendet. Ein besonderes Ansäuern des Ausgangsgutes vor der Extraktion ist meistens nicht erforderlich. Bei der fraktionierten Destillation der in die neutrale Form übergeführten Wirkstoffe konnte neben dem im Hauptpatent beschriebenen neutralen Produkt vom F. z73° (aD = - 3,47°) und dem sauren Produkt vom F. r96° (aD =- 3,I9°) eine neue Substanz vom F. I83° (a-D"= -2830, Endwert in alkoholischer Lösung) in kristalliner Form abgetrennt werden. Dieser neue Stoff zeigt die neue Wirkung im Pflanzentest wie die .schon im Hauptpatent beschriebenen Stoffe; seine Wirksamkeit beträgt 5, I olO Avenaeinheiten pro Gramm. Beispiel z o kg Malz werden gemahlen und in etwa fünf Partien geteilt. Diese werden mit kaltem Wasser extrahiert, und zwar so, daß der am weitesten angereicherte Extrakt einer Partie jeweils mit dem frischesten Material in Berührung kommt. Bei Verwendung von etwa 2o 1 Wasser kann man durch Abheben der überstehenden Flüssigkeit etwa i q. bis 15 1 Extrakt erhalten. Dieser sauer reagierende wäßrige Extrakt wird wiederholt mit peroxydfreiem Äther, insgesamt etwa mit dem gleichen Volumen, ausgeschüttelt. Die ätherische Lösung wird eingeengt und dann mit Bicarbonatlösung ausgeschüttelt. Die wirksame Substanz wird aus der Bicarbonatlösung durch Ansäuern freigemacht, mit Äther aufgenommen und der Rückstand der ätherischen Lösung durch Auskochen' mit Petroläther oder Ligroin von anderen aktiven Begleitstoffen befreit. Die- weitere Reinigung erfolgt nach der im Hauptpatent beschriebenen Arbeitsweise. Bei der Hochvakuumdestillation der bei der Weiterverarbeitung anfallenden neutralen Produkte fängt man das bei i i o bis i20° (Badtemperatur) und o,i mm Druck erhaltene Destillat gesondert auf. Es kristallisiert meist erst nach einigen Tagen, ein Vorgang, der durch Kühlung mit Kohlensäure-Aceton-Mischung beschleunigt werden kann. Die Kristalle werden aus Alkohol-Ligroin (i: i) umkristallisiert und zeigen den Schmelzpunkt i83°.- Die bei höherer Badtemperatur erhaltenen Anteile des Destillats ergeben die im Hauptpatent beschriebenen kristallinischen Wirkstoffe.In further processing of the subject matter of the invention of the main patent it has now been shown that germinated seeds, e.g. B. good malts are a particularly rich starting material for the production of growth hormones, and that these active ingredients can be obtained therefrom in good yield if the procedures specified in the main patent are applied to this starting material. A special acidification of the starting material before the extraction is usually not necessary. In the fractional distillation of the transferred in the neutral form active substances could in addition to the process described in the main patent neutral product, melting at Z73 ° (aD = - 3.47 °) and the acid product from F. r96 ° (aD = - 3, I9 ° ) a new substance with a temperature of I83 ° (aD "= -2830, final value in alcoholic solution) can be separated in crystalline form. This new substance shows the new effect in the plant test like the substances already described in the main patent; its effectiveness is 5, 100 avena units per gram. For example, zo kg of malt are ground and divided into about five lots. These are extracted with cold water in such a way that the most enriched extract of a lot comes into contact with the freshest material About 2o 1 of water can be obtained by lifting off the supernatant liquid from about 1 to 15 liters of extract. This acidic reacting aqueous extract is repeated with peroxide-free ether, a total of about the same volume, shaken out. The ethereal solution is concentrated and then extracted with bicarbonate solution. The active substance is freed from the bicarbonate solution by acidification, absorbed with ether and the residue of the ethereal solution is freed from other active accompanying substances by boiling with petroleum ether or ligroin. The further cleaning takes place according to the procedure described in the main patent. In the high vacuum distillation of the neutral products obtained during further processing, the distillate obtained at 110 to 120 ° (bath temperature) and 0.1 mm pressure is collected separately. It usually only crystallizes after a few days, a process that can be accelerated by cooling with a mixture of carbonic acid and acetone. The crystals are recrystallized from alcohol-ligroin (i: i) and have a melting point of 183 °. The proportions of the distillate obtained at a higher bath temperature give the crystalline active ingredients described in the main patent.

Claims (1)

PATENTANSPRUCH Abänderung des Verfahrens gemäß Patent 586 2q.6,- dadurch gekennzeichnet, daß hier gekeimte Samen als Ausgangsmaterialien zur Anwendung kommen.PATENT CLAIM Modification of the process according to patent 586 2q.6, - thereby characterized in that germinated seeds are used as starting materials here.
DEI47327D 1933-06-01 1933-06-01 Process for the production of growth hormones or their esters Expired DE600400C (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
DEI47327D DE600400C (en) 1933-06-01 1933-06-01 Process for the production of growth hormones or their esters

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DEI47327D DE600400C (en) 1933-06-01 1933-06-01 Process for the production of growth hormones or their esters

Publications (1)

Publication Number Publication Date
DE600400C true DE600400C (en) 1934-07-21

Family

ID=7191968

Family Applications (1)

Application Number Title Priority Date Filing Date
DEI47327D Expired DE600400C (en) 1933-06-01 1933-06-01 Process for the production of growth hormones or their esters

Country Status (1)

Country Link
DE (1) DE600400C (en)

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