CH227706A - Process for the preparation of d (+) - a, y-dioxy-B, B-dimethyl-butyric acid- (3'-oxy-propyl-) amide. - Google Patents

Process for the preparation of d (+) - a, y-dioxy-B, B-dimethyl-butyric acid- (3'-oxy-propyl-) amide.

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Publication number
CH227706A
CH227706A CH227706DA CH227706A CH 227706 A CH227706 A CH 227706A CH 227706D A CH227706D A CH 227706DA CH 227706 A CH227706 A CH 227706A
Authority
CH
Switzerland
Prior art keywords
oxy
dimethyl
dioxy
amide
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 CH227706A publication Critical patent/CH227706A/en

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Classifications

    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C233/00Carboxylic acid amides
    • C07C233/01Carboxylic acid amides having carbon atoms of carboxamide groups bound to hydrogen atoms or to acyclic carbon atoms
    • C07C233/16Carboxylic acid amides having carbon atoms of carboxamide groups bound to hydrogen atoms or to acyclic carbon atoms having the nitrogen atom of at least one of the carboxamide groups bound to a carbon atom of a hydrocarbon radical substituted by singly-bound oxygen atoms

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)

Description

  

  Verfahren zur Darstellung von     d(+)-a,        r-Dioay-ss,        f-dimethyl-uuttersäure-          (3'-ogy-propyl-)amid.       Für die Herstellung der     Pantothensäure     und ihrer Homologen wird     d,(-)-a-Oxy-ss,ss-          dimethyl-y-butyrolactan        mit        ss-Alanin,    seinen  Salzen oder     Estern,    oder mit entsprechenden  andern     Aminoe:arbonsäuren    umgesetzt (siehe  zum     Beispiel        Science,    91 [19403 S. 411;

         Journ.    of     the        Americ.        Chem.   <B>See,</B> 62 [1940]  S. 1785; amerikanisches Patent Nr. 2234680;       Helv.        Chim.    Acta, 23 [19401 S. 651;     Journ.     of     the        Americ.        Chem.        Soc.,    62 [1940]  S. 1628).  



  Es wurde nun gefunden, dass man zu     neuen          A.bkö:mmlingen    der     d(-)-a,y-Dioxy-ss,ss-di-          methyl-buttersäure        gelangt,    wenn man     Al-          kanolamine    auf sie einwirken lässt. Die Um  setzung wird     vorzugsweise    in einem Lösungs  mittel durchgeführt.  



  Gegenstand des vorliegenden Patentes ist  ein Verfahren zur     Darstellung    von     d(+)-a,y-          Dioxy    -     ss,ss    -     dimethyl    -     buttersäure    - (3' -     oxy-          propyl-)-amid,        welches    dadurch gekennzeich  net ist,     da.ss    man d'(-)-a-Oxy-ss,ss-dimethyl-         y-butyrolacto@n    mit     3-Oxy-propylamin    um  setzt.  



  Das bisher     unbekannte    Verfahrenserzeug  nis ist ein     farbloses,        zähflüssiges,    leicht       wasserl:öslich-es    0:1, welches unter 0,02 mm       zwischen    118 und 120  siedet und für c = 3  in     Watssser    eine     spezifische    Drehung von  a     v    =     +    29,7  zeigt.  



  Die neue Verbindung vermag die Wir  kungen der     Pantothensäure        auszuüben    und  soll als     Arzneimittel    Verwendung finden.  



       Beispiel:     Man löst 130 Gewichtsteile     d(-)-a-Oxy-          ss,ss-.dimethyl-y-butyrolacton    in 150     Vo:lum-          teilen    Methylalkohol. Zu der Lösung fügt  man auf einmal 75     Gewichtsteile        3-Oxy-pro-          pylamin    und rührt gut .durch. Die Um  setzung setzt     unter        Selbsterwärmung    ein.  Die Temperatur     steigt    langsam bis gegen  50 . Nach etwa 2     Stunden    beginnt die Tem  peratur wieder zu sinken.

   Um     vollständige              Umsetzung    herbeizuführen, lässt man noch  24 Stunden bei Zimmertemperatur stehen.  Das ,gebildete     d(+)-a,y-Dioxy-ss"B-dimethyl-          buttersäure-        (3'-,oxy-propyl-)amid    wird im  Vakuum vom Methylalkohol befreit. Es       binterbleibt    als farbloses, zähflüssiges, leicht       wasserlösliches    Öl.



  Process for the preparation of d (+) - a, r-Dioay-ss, f-dimethyl-butyric acid- (3'-ogy-propyl-) amide. For the preparation of pantothenic acid and its homologues, d, (-) - a-oxy-ss, ss-dimethyl-y-butyrolactane is reacted with s-alanine, its salts or esters, or with other corresponding amino acids (see for example Science, 91 [19403 p. 411;

         Journ. of the Americ. Chem. See, 62 [1940] p. 1785; American Patent No. 2234680; Helv. Chim. Acta, 23 [19401 p. 651; Journ. of the Americ. Chem. Soc., 62 [1940] p. 1628).



  It has now been found that new types of d (-) - a, y-dioxy-ss, ss-dimethyl-butyric acid can be obtained if alkanolamines are allowed to act on them. The implementation is preferably carried out in a solvent.



  The subject of the present patent is a process for the preparation of d (+) - a, y-dioxy - ss, ss - dimethyl - butyric acid - (3 '- oxy-propyl -) - amide, which is characterized by da.ss one d '(-) - a-oxy-ss, ss-dimethyl-y-butyrolacto @ n with 3-oxy-propylamine to implement.



  The previously unknown process product is a colorless, viscous, slightly water-soluble 0: 1, which boils below 0.02 mm between 118 and 120 and shows a specific rotation of av = + 29.7 for c = 3 in Watssser .



  The new compound is able to exert the effects of pantothenic acid and should be used as a medicinal product.



       Example: 130 parts by weight of d (-) - a-oxy-ss, ss-.dimethyl-y-butyrolactone are dissolved in 150 parts by volume of methyl alcohol. 75 parts by weight of 3-oxypropylamine are added all at once to the solution and the mixture is stirred thoroughly. The implementation begins with self-heating. The temperature rises slowly to around 50. After about 2 hours, the temperature begins to drop again.

   In order to bring about complete conversion, it is left to stand at room temperature for a further 24 hours. The d (+) - a, y-dioxy-ss "B-dimethylbutyric acid (3 '-, oxy-propyl) amide formed is freed from methyl alcohol in vacuo. It remains as a colorless, viscous, easily water-soluble oil .

 

Claims (1)

PATENTANSPRUCH EMI0002.0007 Verfahren <SEP> zur <SEP> Darstellung <SEP> von <SEP> d(+)-a,y Dioxy- <SEP> ss"B-.dim,ethyl <SEP> -buttersäure-(3'-oxy-pro- pyl-)amid, dadurch gekennzeichnet, class man d(-)-a-Oxy-ss',ss-dimethyl-y-butyrolacton mit 3-Oxy-propyla.min umsetzt. Das bisher unbekannte Verfahrenserzeug nis ist ein farbloses, zähfliissiges, leicht wasserlösliches öl, welches unter 0,02 mm zwischen<B>118</B> und 190 siedet und für c = 3 in Wasser eine spezifische Drehung von a @j - + <B>29,7'</B> Zeigt. PATENT CLAIM EMI0002.0007 Method <SEP> for <SEP> representation <SEP> of <SEP> d (+) - a, y Dioxy- <SEP> ss "B-.dim, ethyl <SEP> -butyric acid- (3'-oxy-pro - pyl) amide, characterized in that d (-) - a-oxy-ss', ss-dimethyl-y-butyrolactone is reacted with 3-oxy-propyla.min. The so far unknown process product is a colorless, viscous one , easily water-soluble oil, which boils below 0.02 mm between <B> 118 </B> and 190 and for c = 3 in water a specific rotation of a @j - + <B> 29.7 '</B> Shows.
CH227706D 1943-09-06 1942-05-08 Process for the preparation of d (+) - a, y-dioxy-B, B-dimethyl-butyric acid- (3'-oxy-propyl-) amide. CH227706A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CH227706T 1943-09-06

Publications (1)

Publication Number Publication Date
CH227706A true CH227706A (en) 1943-06-30

Family

ID=4455191

Family Applications (1)

Application Number Title Priority Date Filing Date
CH227706D CH227706A (en) 1943-09-06 1942-05-08 Process for the preparation of d (+) - a, y-dioxy-B, B-dimethyl-butyric acid- (3'-oxy-propyl-) amide.

Country Status (1)

Country Link
CH (1) CH227706A (en)

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