CH200245A - Process for the preparation of the 3-carboxamide of N-arabinosido-dihydropyridine. - Google Patents

Process for the preparation of the 3-carboxamide of N-arabinosido-dihydropyridine.

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Publication number
CH200245A
CH200245A CH200245DA CH200245A CH 200245 A CH200245 A CH 200245A CH 200245D A CH200245D A CH 200245DA CH 200245 A CH200245 A CH 200245A
Authority
CH
Switzerland
Prior art keywords
carboxamide
preparation
arabinosido
dihydropyridine
sep
Prior art date
Application number
Other languages
German (de)
Inventor
F Hoffmann- Aktiengesellschaft
Original Assignee
Hoffmann La Roche
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 Hoffmann La Roche filed Critical Hoffmann La Roche
Publication of CH200245A publication Critical patent/CH200245A/en

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Classifications

    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07HSUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
    • C07H19/00Compounds containing a hetero ring sharing one ring hetero atom with a saccharide radical; Nucleosides; Mononucleotides; Anhydro-derivatives thereof
    • C07H19/02Compounds containing a hetero ring sharing one ring hetero atom with a saccharide radical; Nucleosides; Mononucleotides; Anhydro-derivatives thereof sharing nitrogen
    • C07H19/04Heterocyclic radicals containing only nitrogen atoms as ring hetero atom
    • C07H19/048Pyridine radicals

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Biochemistry (AREA)
  • Biotechnology (AREA)
  • General Health & Medical Sciences (AREA)
  • Genetics & Genomics (AREA)
  • Molecular Biology (AREA)
  • Plural Heterocyclic Compounds (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)

Description

  

  Verfahren zur     Darsteltung    des     3-Carbonsäureamids    des     N-Arabinosido-dihydropyridins.       Es     wurde    gefunden, dass sich aus den  zum     Beispiel    durch Einwirkung von     1-Aceto-          halogenirabinose    und     Nikotins2#ureami@d    in  .einem indifferenten     Lösungsmittel    erhält  lieh-en     3-Carbonsäureami:

  den    der     N-Triacetyl-          a.rabinos.dopyridiniumhalogenide    durch Be  handlung mit     Reduktionsmitteln    in     aJka.-          lischer    Lösung das     3-Carbonsäureamid    des       N-Triacetylarabinosidodihydropyridins.    ge  winnen     lässt,    ohne     ,dass    .dabei der     acylierte     Zuckerrest     irgendwie        verändert    wird.

   Die  entstehende gut     kristallisierende        Dihydrover-          bindung        b.e@itzt    vermutlich folgende     Konsti-          tution     
EMI0001.0029     
         Aus    dem so erhaltenen     @3-Carbonsäureamid          des        N-Triacetylarabinosidodihydropyridins          wird,erfindungsb        mäss    durch Abspaltung der  
EMI0001.0036     
  
    I@ <SEP> I <SEP> i <SEP> i'i <SEP> I <SEP> @I <SEP> I <SEP> @@I            Acetyl@reste    das -     3,

  -Carbonsäureamid    des,     N-          Arabinasidodihydropyridins        hergestellt.     



  Die neue     Verbindung    zersetzt sich ober  halb     IM     , wirkt reduzierend und zeigt in       alkalischer    Lösung ein     Absorptionsmaximum          bei        340,u,u.    .Sie soll     als    Ausgangsstoff für  die     Herstellung    von     Arzneimitteln    dienen.

      <I>Beispiel:</I>       Teile    der Verbindung aus 1-Acetobrom-         arabinose    und     Nikotinsä.ureamid    werden in  50     Teilen        Wasser    gelöst und dazu je 5     Teile          Natriumbicarbonat    und 5 Teile     Natrium-          hydrosulfit    gegeben. Dabei färbt sich die       Lösung    gelb.

   Nach mehrstündigem Stehen       extrahiert    man die     Flüssigkeit    wiederholt       mit        Chloroform    und dampft die     Chloroform-          egtrakte        unter        verminderbem        Druck    ein. Da  bei bleibt das     3-Carbonsäureamid    des       N-Triacetylarabinosidodihydropyridins    als       amorphe        -Masse    zurück.

   Die     Verbindung          reduziert        Silbernitratlösung    in der     Wärme.     Zur Abspaltung .der     Acetylgruppe    löst     mann         sie in     konzentriertem    alkoholischem Am  moniak, lässt acht Stunden bei     Zimmertempe-          ratur        stehen,    verdampft     hierauf        das        Ijö-          sungsmittel    im Vakuum und     kristallisiert     den     Rückstand,

      das     3-Carbonsäureamid    des       N-Arabinosidodihydropyridins    aus etwa  90 %     igem    Alkohol um.



  Process for the preparation of the 3-carboxamide of N-arabinosido-dihydropyridine. It has been found that the 3-carboxylic acid amides obtained, for example, by the action of 1-acetohalogenirabinose and nicotine2 # ureami @ d in an inert solvent:

  that of the N-triacetyl a.rabinos.dopyridinium halide by treatment with reducing agents in aJka.- lischer solution the 3-carboxamide of N-triacetylarabinosidodihydropyridine. can be obtained without the acylated sugar residue being changed in any way.

   The resulting dihydro compound, which crystallizes well, b.e@itzt presumably has the following constitution
EMI0001.0029
         The resulting @ 3-carboxamide of N-triacetylarabinosidodihydropyridine is, according to the invention, by splitting off the
EMI0001.0036
  
    I @ <SEP> I <SEP> i <SEP> i'i <SEP> I <SEP> @I <SEP> I <SEP> @@ I Acetyl @ reste das - 3,

  -Carboxamide des, N-Arabinasidodihydropyridins produced.



  The new compound decomposes above half IM, has a reducing effect and shows an absorption maximum at 340, u, u in alkaline solution. It is intended to serve as a raw material for the manufacture of drugs.

      <I> Example: </I> parts of the compound from 1-acetobromoarabinose and nicotinic acid amide are dissolved in 50 parts of water and 5 parts of sodium bicarbonate and 5 parts of sodium hydrosulfite are added. The solution turns yellow.

   After standing for several hours, the liquid is extracted repeatedly with chloroform and the chloroform extracts are evaporated under reduced pressure. The 3-carboxamide of N-triacetylarabinosidodihydropyridine remains as an amorphous mass.

   The compound reduces silver nitrate solution in the heat. To split off the acetyl group, dissolve it in concentrated alcoholic ammonia, leave it to stand for eight hours at room temperature, then evaporate the solvent in vacuo and crystallize the residue.

      the 3-carboxamide of N-arabinosidodihydropyridine from about 90% alcohol.

 

Claims (1)

PATENTANSPRUCH Verfahren zur Darstellung des 3-Carbon- säureamids des N-Arabinosidodihydropyri- dins, dadurch gekennzeichnet, dass man das 3-Carbonsäureami, PATENT CLAIM Process for the preparation of the 3-carboxylic acid amide of N-arabinosidodihydropyridine, characterized in that the 3-carboxylic acid amide d eines N-Triaoetylarabino- sid opyri-diniumhalogenid in alkalischer Lö sung reduziert und aus dem so erhaltenen Produkt die Aoetylreste abspaltet. Die neue Verbindung zersetzt sich ober halb 165 , d of an N-triaoetylarabinoid opyridinium halide is reduced in alkaline solution and the aoetyl radicals are split off from the product thus obtained. The new compound disintegrates above 165 wirkt reduzierend und zeigt in alkalischer Lösung ein Absorptionsmaximum bei 340,u,u. Sie soll als Ausgangsstoff für die Herstellung von Arzneimitteln dienen. has a reducing effect and shows an absorption maximum at 340, u, u in alkaline solution. It is intended to serve as a raw material for the manufacture of pharmaceuticals.
CH200245D 1936-12-08 1936-12-08 Process for the preparation of the 3-carboxamide of N-arabinosido-dihydropyridine. CH200245A (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CH195950T 1936-12-08
CH200245T 1936-12-08

Publications (1)

Publication Number Publication Date
CH200245A true CH200245A (en) 1938-09-30

Family

ID=25722815

Family Applications (1)

Application Number Title Priority Date Filing Date
CH200245D CH200245A (en) 1936-12-08 1936-12-08 Process for the preparation of the 3-carboxamide of N-arabinosido-dihydropyridine.

Country Status (1)

Country Link
CH (1) CH200245A (en)

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