CH311631A - Process for the production of a new basic substituted fatty acid (2-halogen-6-methyl-anilide). - Google Patents

Process for the production of a new basic substituted fatty acid (2-halogen-6-methyl-anilide).

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Publication number
CH311631A
CH311631A CH311631DA CH311631A CH 311631 A CH311631 A CH 311631A CH 311631D A CH311631D A CH 311631DA CH 311631 A CH311631 A CH 311631A
Authority
CH
Switzerland
Prior art keywords
anilide
methyl
methylamine
halogen
chloro
Prior art date
Application number
Other languages
German (de)
Inventor
Aktiengesellschaft Cilag
Original Assignee
Cilag 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 Cilag Ag filed Critical Cilag Ag
Publication of CH311631A publication Critical patent/CH311631A/en

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Classifications

    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D295/00Heterocyclic compounds containing polymethylene-imine rings with at least five ring members, 3-azabicyclo [3.2.2] nonane, piperazine, morpholine or thiomorpholine rings, having only hydrogen atoms directly attached to the ring carbon atoms
    • C07D295/04Heterocyclic compounds containing polymethylene-imine rings with at least five ring members, 3-azabicyclo [3.2.2] nonane, piperazine, morpholine or thiomorpholine rings, having only hydrogen atoms directly attached to the ring carbon atoms with substituted hydrocarbon radicals attached to ring nitrogen atoms
    • C07D295/14Heterocyclic compounds containing polymethylene-imine rings with at least five ring members, 3-azabicyclo [3.2.2] nonane, piperazine, morpholine or thiomorpholine rings, having only hydrogen atoms directly attached to the ring carbon atoms with substituted hydrocarbon radicals attached to ring nitrogen atoms substituted by carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals
    • 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
    • C07C233/02Carboxylic acid amides having carbon atoms of carboxamide groups bound to hydrogen atoms or to acyclic carbon atoms having nitrogen atoms of carboxamide groups bound to hydrogen atoms or to carbon atoms of unsubstituted hydrocarbon radicals
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C237/00Carboxylic acid amides, the carbon skeleton of the acid part being further substituted by amino groups

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Description

  

  



  Verfahren zur Herstellung eines neuen basisch substituierten   Fettsäure-     (2-halogen-6-methyl-anilids).



   Gegenstand des vorliegenden Patentes bildet ein Verfahren zur Herstellung eines neuen basisch substituierten Fettsäure-(2-halogen-6  methyl-anilids),    welches dadurch   gekennzeich-    net ist, dass man eine Verbindung der Formel
EMI1.1     
 in welcher X einen reaktionsfähigen, während der Reaktion sieh abspaltenden Rest bedeutet, mit Methylamin umsetzt.



   Der Rest X kann in einem Halogenatom oder einem sonstigen f r den Austausch gegen den   basisehen    Rest   geeigneten reaktionsfähi-    gen Substituenten, wie z. B. einer Alkylsulfo  nvloxy-oder Arylsulfonyloxygruppe    bestehen.



  Der Austausch der Gruppe X gegen den Me  thylaminrest    erfolgt z. B. durch einfaches Er  värmen mit hIethylamin    gegebenenfalls in Gegenwart eines basisch reagierenden Konden  sationsmittels    oder von Methylamin im ¯ber  schuss.    Das ¯-Methylamino-propionsÏure-(2  ehlor-6-methyl-anilid)    ist ein   öl,    das nach einiger Zeit zu farblosen Kristallen erstarrt. Das Hydrochlorid der Base schmilzt bei 173, 5 bis   174 .   



   Das neue Anilid soll als   Lokalanästhetikum    und als Zwischenprodukt zur Herstellung weiterer Derivate Verwendmg finden.



   Beispiel :
40 Gewichtsteile ¯-Chlor-propionsÏure-(2  ehlor-6-methyl-anilid)    werden in 100   Gewichts-    teilen Methanol suspendiert und mit 140 Ge  wichtsteilen Methylaminlösung    versetzt. Die Temperatur steigt dabei leicht an, und ein grosser Teil des   Reaktionsgemisehes    geht in Lösung. Nun wird während 4 Stunden bei Zimmertemperatur gerührt und dann einige Stunden unter Druck bei 100-110¯. Mit Wasserdampf wird hierauf der Alkohol und das übersehüssige Methylamin abgeblasen und nach dem Erkalten das zurüekbleibende öl in Äther aufgenommen. Nach dem Trocknen der ätherischen   Losung    und Verjagen des Lösungsmittels verbleibt ein   öl,    das durch Uberführen in das Hydrochlorid gereinigt wird.



  Man erhält 30 Gewichtsteile reines   B-Methyl-    amino-propionsäure- (2-chlor-6-methyl-anilid).



  Die Umsetzung mit Methylamin kann auch in Benzol stattfinden.  



   PATENTANSPRUCH :
Verfahren zur Herstellung eines neuen basisch substituierten   Fettsäure- (2-halogen-6-      methylanilids),    dadurch gekennzeichnet, dass man eine Verbindung der Formel
EMI1.2     
 

**WARNUNG** Ende DESC Feld konnte Anfang CLMS uberlappen**.





  



  Process for the production of a new basic substituted fatty acid (2-halogen-6-methyl-anilide).



   The subject matter of the present patent is a process for the preparation of a new basic substituted fatty acid (2-halogen-6-methyl-anilide), which is characterized in that a compound of the formula
EMI1.1
 in which X denotes a reactive radical which is split off during the reaction, with methylamine.



   The radical X can be in a halogen atom or another reactive substituent suitable for replacement with the basic radical, such as B. an Alkylsulfo nvloxy or Arylsulfonyloxygruppe exist.



  The exchange of group X against the Me thylaminrest takes place z. B. by simply heating it with methylamine, possibly in the presence of a basic condensation agent or of methylamine in excess. The ¯-methylamino-propionic acid (2 chloro-6-methyl-anilide) is an oil that solidifies to colorless crystals after a while. The hydrochloride of the base melts at 173.5-174.



   The new anilide is said to be used as a local anesthetic and as an intermediate for the production of other derivatives.



   Example:
40 parts by weight of ¯-chloropropionic acid (2 chloro-6-methyl-anilide) are suspended in 100 parts by weight of methanol and 140 parts by weight of methylamine solution are added. The temperature rises slightly and a large part of the reaction mixture goes into solution. The mixture is then stirred for 4 hours at room temperature and then for a few hours under pressure at 100-110¯. The alcohol and excess methylamine are then blown off with steam and, after cooling, the remaining oil is absorbed in ether. After the ethereal solution has dried and the solvent has been driven off, an oil remains which is purified by converting it into the hydrochloride.



  30 parts by weight of pure B-methylamino-propionic acid (2-chloro-6-methyl-anilide) are obtained.



  The reaction with methylamine can also take place in benzene.



   PATENT CLAIM:
Process for the preparation of a new basic substituted fatty acid (2-halo-6-methylanilide), characterized in that a compound of the formula
EMI1.2
 

** WARNING ** End of DESC field could overlap beginning of CLMS **.



 

Claims (1)

**WARNUNG** Anfang CLMS Feld konnte Ende DESC uberlappen **. ** WARNING ** Beginning of CLMS field could overlap end of DESC **. Verfahren zur Herstellung eines neuen basisch substituierten Fettsäure- (2-halogen-6-methyl-anilids). Process for the production of a new basic substituted fatty acid (2-halogen-6-methyl-anilide). Gegenstand des vorliegenden Patentes bildet ein Verfahren zur Herstellung eines neuen basisch substituierten Fettsäure-(2-halogen-6 methyl-anilids), welches dadurch gekennzeich- net ist, dass man eine Verbindung der Formel EMI1.1 in welcher X einen reaktionsfähigen, während der Reaktion sieh abspaltenden Rest bedeutet, mit Methylamin umsetzt. The subject matter of the present patent is a process for the preparation of a new basic substituted fatty acid (2-halogen-6-methyl-anilide), which is characterized in that a compound of the formula EMI1.1 in which X denotes a reactive radical which is split off during the reaction, with methylamine. Der Rest X kann in einem Halogenatom oder einem sonstigen f r den Austausch gegen den basisehen Rest geeigneten reaktionsfähi- gen Substituenten, wie z. B. einer Alkylsulfo nvloxy-oder Arylsulfonyloxygruppe bestehen. The radical X can be in a halogen atom or another reactive substituent suitable for replacement with the basic radical, such as B. an Alkylsulfo nvloxy or Arylsulfonyloxygruppe exist. Der Austausch der Gruppe X gegen den Me thylaminrest erfolgt z. B. durch einfaches Er värmen mit hIethylamin gegebenenfalls in Gegenwart eines basisch reagierenden Konden sationsmittels oder von Methylamin im ¯ber schuss. Das ¯-Methylamino-propionsÏure-(2 ehlor-6-methyl-anilid) ist ein öl, das nach einiger Zeit zu farblosen Kristallen erstarrt. Das Hydrochlorid der Base schmilzt bei 173, 5 bis 174 . The exchange of group X against the Me thylaminrest takes place z. B. by simply heating it with methylamine, possibly in the presence of a basic condensation agent or of methylamine in excess. The ¯-methylamino-propionic acid (2 chloro-6-methyl-anilide) is an oil that solidifies to colorless crystals after a while. The hydrochloride of the base melts at 173.5-174. Das neue Anilid soll als Lokalanästhetikum und als Zwischenprodukt zur Herstellung weiterer Derivate Verwendmg finden. The new anilide is said to be used as a local anesthetic and as an intermediate for the production of other derivatives. Beispiel : 40 Gewichtsteile ¯-Chlor-propionsÏure-(2 ehlor-6-methyl-anilid) werden in 100 Gewichts- teilen Methanol suspendiert und mit 140 Ge wichtsteilen Methylaminlösung versetzt. Die Temperatur steigt dabei leicht an, und ein grosser Teil des Reaktionsgemisehes geht in Lösung. Nun wird während 4 Stunden bei Zimmertemperatur gerührt und dann einige Stunden unter Druck bei 100-110¯. Mit Wasserdampf wird hierauf der Alkohol und das übersehüssige Methylamin abgeblasen und nach dem Erkalten das zurüekbleibende öl in Äther aufgenommen. Nach dem Trocknen der ätherischen Losung und Verjagen des Lösungsmittels verbleibt ein öl, das durch Uberführen in das Hydrochlorid gereinigt wird. Example: 40 parts by weight of ¯-chloropropionic acid (2 chloro-6-methyl-anilide) are suspended in 100 parts by weight of methanol and 140 parts by weight of methylamine solution are added. The temperature rises slightly and a large part of the reaction mixture goes into solution. The mixture is then stirred for 4 hours at room temperature and then for a few hours under pressure at 100-110¯. The alcohol and excess methylamine are then blown off with steam and, after cooling, the remaining oil is absorbed in ether. After the ethereal solution has dried and the solvent has been driven off, an oil remains which is purified by converting it into the hydrochloride. Man erhält 30 Gewichtsteile reines B-Methyl- amino-propionsäure- (2-chlor-6-methyl-anilid). 30 parts by weight of pure B-methylamino-propionic acid (2-chloro-6-methyl-anilide) are obtained. Die Umsetzung mit Methylamin kann auch in Benzol stattfinden. The reaction with methylamine can also take place in benzene. PATENTANSPRUCH : Verfahren zur Herstellung eines neuen basisch substituierten Fettsäure- (2-halogen-6- methylanilids), dadurch gekennzeichnet, dass man eine Verbindung der Formel EMI1.2 in welcher X einen reaktionsfähigen, während der Reaktion sich abspaltenden Rest bedeutet, mit Methylamin umsetzt. Das auf diese Weise erhaltene ¯-Methylamino-propionsÏure-(2 ehlor-6-methyl-anilid) bildet ein 61, das nach einiger Zeit zu farblosen Kristallen erstarrt. PATENT CLAIM: Process for the preparation of a new basic substituted fatty acid (2-halo-6-methylanilide), characterized in that a compound of the formula EMI1.2 in which X is a reactive radical which is split off during the reaction, reacts with methylamine. The ¯-methylamino-propionic acid (2-chloro-6-methyl-anilide) obtained in this way forms a 61 that solidifies to colorless crystals after a while. Das Hydrochlorid der Base schmilzt bei 173, 5 bis 174, 5 . The hydrochloride of the base melts at 173.5 to 174.5. Das neue Anilid soll a. ls LokalanÏsthetikum und als Zwischenprodukt Verwendung finden. The new anilide should a. Can be used as a local anÏesthetic and as an intermediate product. UNTERANSPBrCH : Verfahren naeh Patentanspruch, dadurch gekennzeichnet, dass man ein ¯-Halogen-pro pionsÏure-(2-chlor-6-methyl-anilid) mit Me thylamin reagieren lϯt. SUBSCRIBE: Process according to patent claim, characterized in that a ¯-halogen-propionic acid (2-chloro-6-methyl-anilide) is allowed to react with methylamine.
CH311631D 1952-02-25 1952-02-25 Process for the production of a new basic substituted fatty acid (2-halogen-6-methyl-anilide). CH311631A (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CH311631T 1952-02-25
CH307799T 1952-11-25

Publications (1)

Publication Number Publication Date
CH311631A true CH311631A (en) 1955-11-30

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CH311631D CH311631A (en) 1952-02-25 1952-02-25 Process for the production of a new basic substituted fatty acid (2-halogen-6-methyl-anilide).

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CH (1) CH311631A (en)

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