DE748459C - Process for the preparation of ketones of 2- (ª ‰ -pyridyl) -pyrroles - Google Patents

Process for the preparation of ketones of 2- (ª ‰ -pyridyl) -pyrroles

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Publication number
DE748459C
DE748459C DET54335D DET0054335D DE748459C DE 748459 C DE748459 C DE 748459C DE T54335 D DET54335 D DE T54335D DE T0054335 D DET0054335 D DE T0054335D DE 748459 C DE748459 C DE 748459C
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DE
Germany
Prior art keywords
nicotine
pyridyl
ketones
pyrroles
preparation
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
DET54335D
Other languages
German (de)
Inventor
Dr Phil Werner Dobke
Dr-Ing Friedrich Keil
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 filed Critical
Priority to DET54335D priority Critical patent/DE748459C/en
Application granted granted Critical
Publication of DE748459C publication Critical patent/DE748459C/en
Expired legal-status Critical Current

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Classifications

    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D401/00Heterocyclic compounds containing two or more hetero rings, having nitrogen atoms as the only ring hetero atoms, at least one ring being a six-membered ring with only one nitrogen atom
    • C07D401/02Heterocyclic compounds containing two or more hetero rings, having nitrogen atoms as the only ring hetero atoms, at least one ring being a six-membered ring with only one nitrogen atom containing two hetero rings
    • C07D401/04Heterocyclic compounds containing two or more hetero rings, having nitrogen atoms as the only ring hetero atoms, at least one ring being a six-membered ring with only one nitrogen atom containing two hetero rings directly linked by a ring-member-to-ring-member bond

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Plural Heterocyclic Compounds (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)

Description

Verfahren zur Herstellung von Ketonen der 2-(ß-Pyridyl)-pyrrole Das Nikotin ist bekanntlich ein starkes Nervengift und seine Verwendung in der Therapie ist daher weitgehend eingeschränkt geblieben.Process for the preparation of ketones of 2- (ß-pyridyl) -pyrroles Das Nicotine is known to be a powerful neurotoxin and its use in therapy has therefore remained largely restricted.

Es wurde nun gefunden, daß man zu wertvollen Arzneimitteln von geringer Toxizität gelangt, wenn man das in bekannter Weise zunächst zum Pyrrolderivat- dehydrierte Nikotin bzw. nor-\ il:otin durch Behandlung mit acvlierenden 'Mitteln in pyridvIsubstituierte PN"rrolketone überführt. Beispiele r. \or-Nilcotin wird bei einer Temperatur von etwa 26o0 über Palladiuniasbest geleitet Lind (las erhaltene Katalvsat durch sechsstün- diges Kochen mit Prol)Ionsäure@inlivdrid und atriunipropionat in das 2- (ß- l'yridyl)- 3-liropionvlliN.rrol übergeführt. a. L`ber einen Kontakt, der aus einem Ge- inisch von etwa gleichen Teilen voluminöser Kieselsäure und lletalloxvden. wie z. B. Zinkoxyd, Bariunioxyd, Eisenoxyd, letztere vorteilhafterweise im Gemisch miteinander, besteht, werden bei einer Temperatur von etwa 4oo° die Dämpfe des Nikotins geleitet. Der \ ikotindampfstroni wird gegebenenfalls mit Hilfe eines inerten Gases so geregelt, da!.) nach Austritt der Dämpfe aus der Kontakt- zone kein -Nikotin mehr nachweisbar ist. Das Delivdrierungsprodukt wird alsdann in Essig# säureanhydrid gelöst und nach Zusatz von 1Tatr iuniacetat mehrere Stunden am Rück- lußkühler erhitzt. '?ach Abdestillieren des Essirsäureanlivdri(ls wird aus dein Rück- tand durch Ürnkristallisieren aus Wasser das 2-(E@-F'yridyl)-5-acetvl-@ -nieth\'lp@'i"rol gewonnen. Die Delwdrierung einer Verbindung (leg Nikotinreihe zur entsprechenden \ icotyrin- \"erhindung ist bereits bekannt. Auch die Ac1"lierun; von Pyrrolverbindungen ist an .ach nicht besonders eigenartig. Der patent- begründende, Fortschritt (les neuen 1"(#rfalt- rens besteht jedoch darin, daß seine Erzeugnisse wertvolle Heilmittel sind. So besitzt z. D. (las gernälj Beispiel I erhältliche 2-I jl-Pyridyl )-;-propionylpyrrol eine gegenüber dem Nikotin wesentlich geringere Giftigkeit and zeigt bereits in Dosen von 1.5 mg je ioo g Maus deutliche sedative und bei etwa höheren Dosen sogar schwach narkotische I;igeit;cliaften. so rlal''i das Produkt ausgezeichnet als Sedativum in der Therapie verwendet werden dann. Gegenüber den aus f vrrol gewonnenen Acvlverbindungen haben die Verfahrensprodukte den Vorteil, dar sie infolge der basischen Pyridylgruppe als Salze bedeutend leichter wasserlöslich sind als die #'ewöhniichen Ac@.lln-rrole, die eher sauren als basischen Charakter besitzen und infolgedessen keine Salze zti bilden vermögen. So kann man nach dem neuen Verfahren ohne weiteres so hochprozentige Lösungen herstellen. daLi an der Ratte eine narkotische A'irkung erzielt wird; die bekannten Acylpyrrole müssen clagegen wegen ihrer schweren Löslichkeit in Forin hochprozentiger Emulsionen angewandt werden. Dies ist natürlich für die Therapie ein erheblicher Sachteil gegenüber der Verwendung klarer wässeriger Lösungen.It has now been found that valuable medicaments of low toxicity can be obtained if nicotine or norotine, dehydrated in a known manner, is converted into pyrrole-substituted PN ketones by treatment with activating agents. Examples r. \ or-Nilcotine is made at a temperature from about 26o0 passed through Palladiuniasbest Lind (read the received catalog for six hours diges boiling with Prol) Ionsäure @ inlivdrid and atriunipropionat into the 2- (ß- l'yridyl) - 3-liropionvlliN.rrol transferred. a. About a contact that comes from a inically more voluminous by roughly equal parts Silicic acid and metal oxide. such as B. Zinc oxide, barium oxide, iron oxide, the latter advantageously mixed with one another, exist at a temperature of about 400 ° the vapors of the nicotine passed. The \ ikotindampfstroni is if necessary regulated with the help of an inert gas, there!) after the vapors have escaped from the contact zone, nicotine is no longer detectable. That The product is then poured into vinegar acid anhydride dissolved and after the addition of 1Tatrium acetate several hours on the back Heated fluid cooler. '? oh distilling off the Acid anlivdri (ls is made from your back It was made by crystallizing from water the 2- (E @ -F'yridyl) -5-acetyl- @ -nieth \ 'lp @' i "rol won. The twisting of a compound (leg Nicotine series for the corresponding \ icotyrin- \ "Your invention is already known. Also the Ac1 "lierun; of pyrrole compounds is on After all, not particularly strange. The patent reasoning, progress (les new 1 "(# rfalt- rens is, however, that its products are valuable medicinal products. So has z. D. (read like Example I available 2-I jl-pyridyl) -; - propionylpyrrole a significantly lower toxicity compared to nicotine and shows already in doses of 1.5 mg per 100 g mouse clear sedative and at higher doses even slightly narcotic I; igeit; cliaften. so rlal''i the product can then be used excellent as a sedative in therapy. The products of the process have the advantage over the acrylic compounds obtained from molar that, because of the basic pyridyl group, they are significantly more soluble in water as salts than the usual acoln-ols, which are more acidic than basic and consequently do not form any salts capital. So you can easily produce such high-percentage solutions using the new process. that a narcotic effect is achieved in the rat; the known acylpyrroles, on the other hand, have to be used because of their poor solubility in high-percentage emulsions. This is of course a significant factual aspect for therapy compared to the use of clear aqueous solutions.

Claims (1)

PATRNTAVSPRUCII:
Verfahren zur Herstellung von 2-1 1i- Pvridvl)-p@-: cvllcetonen, dadurch gekenn- zeichnet, dar man das in bekannter Weise delivdrierte Nicotin bzw. nor--Nicotin im Pvrrolkern in an sich üblicher Weisu acv- liert.
Zur Abgrenzung des _@nme@duug:;,#rgcn- standes vorn Stand der Technik sind im Er- teilungsverfahren folgende Druckschriften in Betracht gezogen worden: Beilsteins Handbuch der organischen ! mie. 4.. _1uf1., Berlin I935 1>%w. 1936. I'd. <XI, S. 271 ff.; B(l. 11III. S. I8,,: Chemisches Zentralblatt 1c)28 1I S. 20)7 tind 1929 11 S. ?033; Berichte der Deutschen Cheini:chen t_@e:ell- schaft, 13d. 16, S. a3-18.
PATRNTAVSPRUCII:
Method of making 2-1 1i- Pvridvl) -p @ -: cvllcetonen, thus marked- draws that in a familiar way delivered nicotine or nor - nicotine im Pvrrolkern in per se usual manner acv- lates.
To delimit the _ @ nme @ duug:;, # rgcn- state-of-the-art technology are being developed the following publications in Considered: Beilstein's Handbook of Organic! mie. 4 .. _1uf1., Berlin 1935 1>% w. 1936. I'd. <XI, p. 271 ff .; B ( l. 11III. P. 18 ,,: Chemisches Zentralblatt 1c) 28 1I p. 20) 7 tind 1929 11 p. 0 33; Reports of the German Cheini: chen t_ @ e: ell- shank, 13d. 16, pp. A3-18.
DET54335D 1940-10-09 1940-10-09 Process for the preparation of ketones of 2- (ª ‰ -pyridyl) -pyrroles Expired DE748459C (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
DET54335D DE748459C (en) 1940-10-09 1940-10-09 Process for the preparation of ketones of 2- (ª ‰ -pyridyl) -pyrroles

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DET54335D DE748459C (en) 1940-10-09 1940-10-09 Process for the preparation of ketones of 2- (ª ‰ -pyridyl) -pyrroles

Publications (1)

Publication Number Publication Date
DE748459C true DE748459C (en) 1944-11-03

Family

ID=7564363

Family Applications (1)

Application Number Title Priority Date Filing Date
DET54335D Expired DE748459C (en) 1940-10-09 1940-10-09 Process for the preparation of ketones of 2- (ª ‰ -pyridyl) -pyrroles

Country Status (1)

Country Link
DE (1) DE748459C (en)

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
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