DE1058999B - Process for the preparation of a coccidiosis agent - Google Patents

Process for the preparation of a coccidiosis agent

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Publication number
DE1058999B
DE1058999B DEN13415A DEN0013415A DE1058999B DE 1058999 B DE1058999 B DE 1058999B DE N13415 A DEN13415 A DE N13415A DE N0013415 A DEN0013415 A DE N0013415A DE 1058999 B DE1058999 B DE 1058999B
Authority
DE
Germany
Prior art keywords
dimethyl
hydroxypyrimidine
compound
preparation
molecular compound
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.)
Pending
Application number
DEN13415A
Other languages
German (de)
Inventor
Gabriel Gever
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.)
Warner Chilcott Pharmaceuticals Inc
Original Assignee
Norwich Pharmacal Co
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 Norwich Pharmacal Co filed Critical Norwich Pharmacal Co
Publication of DE1058999B publication Critical patent/DE1058999B/en
Pending legal-status Critical Current

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Classifications

    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D307/00Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
    • C07D307/02Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings
    • C07D307/34Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members
    • C07D307/56Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
    • C07D307/70Nitro radicals
    • C07D307/71Nitro radicals attached in position 5
    • C07D307/72Nitro radicals attached in position 5 with hydrocarbon radicals, substituted by nitrogen-containing radicals, attached in position 2
    • C07D307/74Nitro radicals attached in position 5 with hydrocarbon radicals, substituted by nitrogen-containing radicals, attached in position 2 by hydrazino or hydrazono or such substituted radicals
    • C07D307/76Nitro radicals attached in position 5 with hydrocarbon radicals, substituted by nitrogen-containing radicals, attached in position 2 by hydrazino or hydrazono or such substituted radicals having carbonic acyl radicals or their thio or nitrogen analogues directly attached to the hydrazino or hydrazono radical, e.g. semicarbazides

Description

Verfahren zur Herstellung eines. Coccidiosemittels Es wurde gefunden, daß man durch Umsetzung von 4,6-Dimethyl-2-hydroxy-pyrimidin mit 5-NitrofÜrfürolsemicarbazon eine Molekülverbindung der folgenden Formel erhält Diese neue Verbindung ist ein stark wirksames Mittel gegen Coccidiose, eine weit verbreitete und gefährliche Kükenkrankheit, welche eine der schwersten Gefahren für die Geflügelzucht darstellt. Verabreicht man Küken, die mit 500 000 Oocysten von Eimeria tenella infiziert worden waren, die neue Molekülverbindung in Dosen von etwa 15 mg/kg über einen Zeitraum von weniger als einer Woche, so überleben 90 bis 100 % der Hühner diese Infektion; beim Kontrollversuch (gleiche Infektion, aber keine Behandlung mit der Verbindung gemäß vorliegender Erfindung) starben 80 % der Tiere.Method of making a. Coccidiosis agent It has been found that a molecular compound of the following formula is obtained by reacting 4,6-dimethyl-2-hydroxypyrimidine with 5-NitrofUrfürolsemicarbazon This new compound is a potent remedy for coccidiosis, a widespread and dangerous chick disease that is one of the most serious threats to poultry farming. If chicks infected with 500,000 oocysts of Eimeria tenella are administered the new molecular compound in doses of about 15 mg / kg for a period of less than a week, 90 to 100 % of the chickens survive this infection; in the control experiment (same infection, but no treatment with the compound according to the present invention) 80 % of the animals died.

Es ist bekannt, daß 4,6-Dimethyl-2-hydroxypyrimidin mit gewissen Carbaniliden Molekülverbindungen bildet. Diese Reaktionsweise des 4,6-Dimethyl-2-hydroxypyrimidins hat jedoch keine allgemeine Gültigkeit, da nicht alle Harnstoffderivate, z. B. 4,4'-Dichlorcarbanilid, Carbanilid, p-Chlorphenylhamstoff und Phenylharnstoff, mit dieser Pyrimidinverbindung reagieren (vgl. Science, Bd. 122 [1955], S. 245). Es ist ferner bekannt, daß einige der aus 4,6-Dimethyl-2-hydroxypyrimidin und Carbaniliden gebildeten Molekülverbindungen (z. B. die 4,4'-Dinitrocarbanilidverbindung gemäß der USA.-Patentschrift 2 731382) coccidiostatische Eigenschaften besitzen. Wie ebenfalls aus »Sciencea, Bd. 122 [1955], S. 245, hervorgeht, sind jedoch nicht alle dem Verfahrensprodukt analogen Molekülverbindungen in gleicher Weise wirksam. Es war daher nicht vorauszusehen, daß die Molekülverbindung aus 4,6-Dimethyl-2-hydroxypyrimidin und 5-INTitrofurfurolsemicarbazon coccidiostatische Eigenschaften besitzt.It is known that 4,6-dimethyl-2-hydroxypyrimidine forms molecular compounds with certain carbanilides. However, this mode of reaction of 4,6-dimethyl-2-hydroxypyrimidine has no general validity, since not all urea derivatives, e.g. B. 4,4'-dichlorocarbanilide, carbanilide, p-chlorophenylurea and phenylurea, react with this pyrimidine compound (cf. Science, Vol. 122 [1955], p. 245). It is also known that some of the molecular compounds formed from 4,6-dimethyl-2-hydroxypyrimidine and carbanilides (e.g. the 4,4'-dinitrocarbanilide compound according to US Pat. No. 2,731,382) have coccidiostatic properties. As can also be seen from Sciencea, Vol. 122 [1955], p. 245, not all molecular compounds analogous to the process product are effective in the same way. It was therefore not foreseeable that the molecular compound of 4,6-dimethyl-2-hydroxypyrimidine and 5-INTitrofurfurolsemicarbazon would have coccidiostatic properties.

Vergleichsversuche, welche mit der verfahrensgemäß hergestellten Verbindung und der 1Vlolekülverbindung aus 4,6-Dimethyl-2-hydroxypyrimidin und 4,4'-Dinitrocarbanilid durchgeführt wurden, haben folgendes ergeben Verabreicht man mit Eimeria tenella infizierten Küken die genannten Verbindungen in einer Konzentration von jeweils 0,0055 bis 0,0125% im Futter, so beträgt die Überlebensrate bei beiden Versuchsreihen etwa 48 bis ,96"/,; beim Kontrollversuch starben 660/, der Tiere. Die Wirksamkeit der beiden Verbindungen gegenüber Eimeria tenella ist demnach etwa gleich. Während die Dinitrocarbanilid - 4,6 - Dimethyl - 2 - hydroxypyrimidin-Molekülverbindung jedoch nur spezifisch gegenüber den verschiedenen Eimeria-Arten wirkt, besitzt die neue Verbindung darüber hinaus ein breites antibakterielles Spektrum; sie ist demnach in der Lage, die bei der Coccidiose (durch Verletzungen des Darm-Epithels) auftretenden Sekundärinfektionen zu verhindern bzw. weitgehend hintanzuhalten.Comparative experiments which were carried out with the compound prepared according to the method and the molecular compound of 4,6-dimethyl-2-hydroxypyrimidine and 4,4'-dinitrocarbanilide have shown the following , 0055 to 0.0125% in the feed, the survival rate in both test series is about 48 to .96 "/,; in the control experiment 660 /, of the animals died. The effectiveness of the two compounds against Eimeria tenella is therefore about the same Dinitrocarbanilide - 4,6 - dimethyl - 2 - hydroxypyrimidine molecular compound only has a specific effect on the various Eimeria species, the new compound also has a broad antibacterial spectrum; it is therefore able to act in coccidiosis (by injuries to the Intestinal epithelium) occurring secondary infections to be prevented or largely prevented.

Die Verabreichung des Verfahrensproduktes an Küken kann in einfacher Weise durch Vermischen mit dem Futter erfolgen. Beiden wirksamenDosen (etwa 15mg/kg) konnten keine schädlichen Nebenwirkungen festgestellt werden. Insbesondere treten bei Verabfolgung der 5 - Nitrofurfurolsemicarbazon- 4,6 - Dimethyl- 2 -hydroxypyrimidin-Molekülverbindung keine Verfärbung derEierschalen und keine Verminderung der Eierproduktion ein, wie sie bei Verabreichung der Dinitrocarbanilid-4,6-Dimethyl-2-hydroxypyrimidin-Molekülverbindung an eierlegende Hühner beobachtet wurden (vgl. Poultry Science, Bd. 36 [1957], S. 880 bis 884). Bei einer geringen Überdosis der erfindungsgemäßen Verbindung - welche sich infolge der schwierigen Kontrolle der Futteraufnahme praktisch nicht sicher vermeiden läßt - wird keine so große Beeinträchtigung der Gewichtszunahme von Küken beobachtet wie bei der entsprechenden Überdosierung der Dinitrocarbanilid-4,6-Dimethyl-2-hydroxypyrimidin-Molekülverbindung (vgl. Poultry Science, Bd. 36 [1957], S. 304 bis 312).The administration of the process product to chicks can be carried out in a simple manner Way by mixing it with the feed. Both effective doses (around 15mg / kg) no harmful side effects could be found. In particular, kick when the 5-nitrofurfurol semicarbazone-4,6-dimethyl-2-hydroxypyrimidine molecule compound is administered no discoloration of the eggshells and no reduction in egg production, such as when the dinitrocarbanilide-4,6-dimethyl-2-hydroxypyrimidine molecular compound is administered have been observed on egg-laying chickens (cf. Poultry Science, Vol. 36 [1957], p. 880 to 884). With a small overdose of the compound according to the invention - which are practically unsure because of the difficult control of feed intake Avoid - will not affect the weight gain of chicks as much observed as with the corresponding overdose of the dinitrocarbanilide-4,6-dimethyl-2-hydroxypyrimidine molecular compound (see Poultry Science, Vol. 36 [1957], pp. 304 to 312).

Die Herstellung der erfindungsgemäßen Molekülverbindung erfolgt in an sich bekannter Weise durch Umsetzung von 4,6-Dimethyl-2-hydroxypyrimidin mit 5-Nitrofurfurolsemicarbazon in geeigneten Lösungsmitteln (z. B. Benzol, Dimethylsulfoxyd und insbesondere Me- :hanol). Nach mehrstündigem (2 bis 16 Stunden) Vex -ühren der Komponenten bei Raumtemperatur kann die ;ebildete feste Molekülverbindung abgetrennt werden. Die Reaktionspartner 4,6-Dimethyl-2-hydroxypyrimidin md 5-Nitrofurfurolsemicarbazon werden vorzugsweise im YIolverhältnis 4:2,5-umgesetzt; die Ausbeute ist dann praktisch quantitativ, während sie bei Anwendung äqui- molekularer Mengen der Reaktionspartner niedriger liegt (etwa 70 °/o der Theorie). Beispiel Ein Gemischaus 5 g 46-Dimethyl-2-hydroxypyrimidin, 5 g 5-Nitrofurfurölsemicarbazon und 25 ccm Methanol wird bei Raumtemperatur 7 Stunden lang gerührt. Das entstandene Produkt wird abfiltriert und getrocknet, wobei 7,9 g der Molekülverbindung erhalten werden; Schmelzpunkt 215°C (Zersetzung). Eil = 486 bei 3750 A. The molecular compound according to the invention is prepared in a manner known per se by reacting 4,6-dimethyl-2-hydroxypyrimidine with 5-nitrofurfurolsemicarbazone in suitable solvents (e.g. benzene, dimethyl sulfoxide and, in particular, methylene : hanol). After several hours (2 to 16 hours) of Vex -guiding the components at room temperature can the ; e formed solid molecular compound are separated. The reactants 4,6-dimethyl-2-hydroxypyrimidine md 5-Nitrofurfurolsemicarbazon are preferably im Yol ratio 4: 2.5 reacted; the yield is then practically quantitative, while when applied they are equi- molecular amounts of the reactants is lower (about 70% of theory). example A mixture of 5 g of 46-dimethyl-2-hydroxypyrimidine, 5 g of 5-nitrofurfur oil semicarbazone and 25 cc of methanol is stirred at room temperature for 7 hours. The resulting product is filtered off and dried, whereby 7.9 g of the molecular compound are obtained; Melting point 215 ° C (decomposition). Express = 486 at 3750 A.

Claims (1)

PATENTANSPRUCH: Verfahren zur Herstellung eines Coccidiosemittels, dadurch gekennzeichnet, daB 4,6-Dimethyl-2-hydroxypyrimidin und '5-Nitrofurfurolsemicarbazon in einem geeigneten Lösungsmittel zu der Molekülverbindung der Formel umgesetzt werden. In Betracht gezogene Druckschriften: -USA.-Patentschrift Nr..2 731382; _ Yournal of the Chemical Sociefy,1953,.S. 1725 bis 1.730.Claim: Process for the production of a coccidiosis agent, characterized in that 4,6-dimethyl-2-hydroxypyrimidine and 5-nitrofurfurolsemicarbazone in a suitable solvent to the molecular compound of the formula implemented. References contemplated: United States Patent No. 2 731382; _ Yournal of the Chemical Society, 1953, p. 1725 to 1.730.
DEN13415A 1956-04-05 1957-03-14 Process for the preparation of a coccidiosis agent Pending DE1058999B (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
US1058999XA 1956-04-05 1956-04-05

Publications (1)

Publication Number Publication Date
DE1058999B true DE1058999B (en) 1959-06-11

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DE (1) DE1058999B (en)

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2731382A (en) * 1954-12-29 1956-01-17 Merck & Co Inc Pyrimidine substituted urea complexes and processes for preparing the same

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2731382A (en) * 1954-12-29 1956-01-17 Merck & Co Inc Pyrimidine substituted urea complexes and processes for preparing the same

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