CH311632A - 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
CH311632A
CH311632A CH311632DA CH311632A CH 311632 A CH311632 A CH 311632A CH 311632D A CH311632D A CH 311632DA CH 311632 A CH311632 A CH 311632A
Authority
CH
Switzerland
Prior art keywords
anilide
butylamine
methyl
chloro
radical
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 CH311632A publication Critical patent/CH311632A/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 basiseh 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,   wäh-    rend der Reaktion sich abspaltenden Rest bedeutet, mit n-Butylamin umsetzt.



   Der Rest X kann in einem Halogenatom oder einem sonstigen für den Austausch gegen den basischen Rest geeigneten reaktionsfähigen Substituenten, wie z. B. einer Alkylsulfonyloxy-oder   Arylsulfonyloxygruppe    bestehen.



  Der Austausch der Gruppe X gegen den n Butylaminrest erfolgt z. B. durch einfaches Erwärmen mit n-Butylamin gegebenenfalls in Gegenwart eines basisch reagierenden Kondensationsmittels oder von n-Butylamin    im Überschuss. Das/ ?-n-Butylamino-propion-      säure- (2-chlor-6-methyl-anilid)    ist ein   61,    das nach einiger Zeit zu farblosen Kristallen erstarrt. Das Hydrochlorid der Base schmilzt bei   223-223,      5 .   



   Das neue Anilid soll als   Lokalanästhetikum    und als   Zwisehenprodukt    zur   Herstellmg    weitere-r Derivate Verwendung finden.



   Beispiel :
40 Gewichtsteile   ?-Chlor-propionsäure-    (2  chlor-6-methyl-anilid)    werden in 200   Gewichts-    teilen Methanol suspendiert und mit 100 Gewichtsteilen n-Butylamin versetzt. Die   Tem-    peratur steigt dabei leicht an, und ein grosser Teil des Reaktionsgemisches geht in   Losung.   



  Nun wird während 4 Stunden bei   Zimmer-    temperatur gerührt und dann einige Stunden bei   100 .    Mit Wasserdampf wird hierauf der Alkohol und das übersehüssige n-Butylamin abgeblasen und nach dem Erkalten das zu  rückbleibende      61    in Äther aufgenommen. Nach dem Trocknen der ätherischen Lösung und   Verjagen    des Lösungsmittels verbleibt ein   öl,    das nach kurzer Zeit erstarrt. Man erhält 48 Gewichtsteile reines   8-n-Butylamino-pro-      pionsäure-      (2-chlor-6-methyl-anilid).    Die Umsetzung mit n-Butylamin kann auch in Benzol stattfinden.  



   PATENTANSPRUCH :
Verfahren zur Herstellung eines neuen basisch substituierten Fettsäure-(2-halogen-6methyl-anilids), 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 of the present patent is a process for the preparation of a new basic substituted fatty acid (2-halo-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, reacts with n-butylamine.



   The radical X can be in a halogen atom or any other reactive substituent suitable for replacement with the basic radical, such as. B. an alkylsulfonyloxy or arylsulfonyloxy group.



  The exchange of group X against the n-butylamine radical takes place, for. B. by simply heating with n-butylamine, optionally in the presence of a basic condensing agent or n-butylamine in excess. The /? -N-Butylamino-propionic acid- (2-chloro-6-methyl-anilide) is a 61 that solidifies to colorless crystals after a while. The base hydrochloride melts at 223-223.5.



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



   Example:
40 parts by weight of? -Chloropropionic acid- (2 chloro-6-methyl-anilide) are suspended in 200 parts by weight of methanol, and 100 parts by weight of n-butylamine 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 at 100. The alcohol and the excess n-butylamine are then blown off with steam and, after cooling, the 61 remaining is taken up in ether. After the essential solution has dried and the solvent has been driven off, an oil remains that solidifies after a short time. 48 parts by weight of pure 8-n-butylamino-propionic acid (2-chloro-6-methyl-anilide) are obtained. The reaction with n-butylamine can also take place in benzene.



   PATENT CLAIM:
Process for the preparation of a new basic substituted fatty acid (2-halo-6methyl-anilide), 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 basiseh 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, wäh- rend der Reaktion sich abspaltenden Rest bedeutet, mit n-Butylamin umsetzt. The subject of the present patent is a process for the preparation of a new basic substituted fatty acid (2-halo-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, reacts with n-butylamine. Der Rest X kann in einem Halogenatom oder einem sonstigen für den Austausch gegen den basischen Rest geeigneten reaktionsfähigen Substituenten, wie z. B. einer Alkylsulfonyloxy-oder Arylsulfonyloxygruppe bestehen. The radical X can be in a halogen atom or any other reactive substituent suitable for replacement with the basic radical, such as. B. an alkylsulfonyloxy or arylsulfonyloxy group. Der Austausch der Gruppe X gegen den n Butylaminrest erfolgt z. B. durch einfaches Erwärmen mit n-Butylamin gegebenenfalls in Gegenwart eines basisch reagierenden Kondensationsmittels oder von n-Butylamin im Überschuss. Das/ ?-n-Butylamino-propion- säure- (2-chlor-6-methyl-anilid) ist ein 61, das nach einiger Zeit zu farblosen Kristallen erstarrt. Das Hydrochlorid der Base schmilzt bei 223-223, 5 . The exchange of group X against the n-butylamine radical takes place, for. B. by simply heating with n-butylamine, optionally in the presence of a basic condensing agent or n-butylamine in excess. The /? -N-Butylamino-propionic acid- (2-chloro-6-methyl-anilide) is a 61 that solidifies to colorless crystals after a while. The base hydrochloride melts at 223-223.5. Das neue Anilid soll als Lokalanästhetikum und als Zwisehenprodukt zur Herstellmg weitere-r Derivate Verwendung finden. The new anilide is to be used as a local anesthetic and as an intermediate product for the production of other derivatives. Beispiel : 40 Gewichtsteile ?-Chlor-propionsäure- (2 chlor-6-methyl-anilid) werden in 200 Gewichts- teilen Methanol suspendiert und mit 100 Gewichtsteilen n-Butylamin versetzt. Die Tem- peratur steigt dabei leicht an, und ein grosser Teil des Reaktionsgemisches geht in Losung. Example: 40 parts by weight of? -Chloropropionic acid- (2 chloro-6-methyl-anilide) are suspended in 200 parts by weight of methanol, and 100 parts by weight of n-butylamine are added. The temperature rises slightly and a large part of the reaction mixture goes into solution. Nun wird während 4 Stunden bei Zimmer- temperatur gerührt und dann einige Stunden bei 100 . Mit Wasserdampf wird hierauf der Alkohol und das übersehüssige n-Butylamin abgeblasen und nach dem Erkalten das zu rückbleibende 61 in Äther aufgenommen. Nach dem Trocknen der ätherischen Lösung und Verjagen des Lösungsmittels verbleibt ein öl, das nach kurzer Zeit erstarrt. Man erhält 48 Gewichtsteile reines 8-n-Butylamino-pro- pionsäure- (2-chlor-6-methyl-anilid). Die Umsetzung mit n-Butylamin kann auch in Benzol stattfinden. The mixture is then stirred for 4 hours at room temperature and then for a few hours at 100. The alcohol and the excess n-butylamine are then blown off with steam and, after cooling, the 61 remaining is taken up in ether. After the essential solution has dried and the solvent has been driven off, an oil remains that solidifies after a short time. 48 parts by weight of pure 8-n-butylamino-propionic acid (2-chloro-6-methyl-anilide) are obtained. The reaction with n-butylamine can also take place in benzene. PATENTANSPRUCH : Verfahren zur Herstellung eines neuen basisch substituierten Fettsäure-(2-halogen-6methyl-anilids), dadurch gekennzeichnet, dass man eine Verbindung der Formel EMI1.2 in welcher X einen reaktionsfähigen, wÏhrend der Reaktion sich abspaltenden Rest bedeu- tet, mit n-Butylamin umsetzt. Das auf diese Weise erhaltene ¯-n-Butylamino-propionsÏure (2-chlor-6-methyl-anilid bildet ein Íl, das nach einiger Zeit zu farblosen Kristallen erstarrt. PATENT CLAIM: Process for the preparation of a new basic substituted fatty acid (2-halo-6methyl-anilide), characterized in that a compound of the formula EMI1.2 in which X means a reactive radical that is split off during the reaction, reacts with n-butylamine. The ¯-n-butylamino-propionic acid (2-chloro-6-methyl-anilide obtained in this way) forms an oil that solidifies after a while to form colorless crystals. Das Hydroehlorid der Base schmilzt bei 223 bis 223, 5o. The hydrochloride of the base melts at 223 to 223.5o. Das neue Anilid soll als Lokalanästhetikum und als Zwischenprodukt Verwendung finden. The new anilide will be used as a local anesthetic and as an intermediate product. UNTERANSPRUCH : Verfahren nach Patentanspruch, dadurch gekennzeichnet da¯ man ein ¯-Halogen-pro pionsÏure-(2-chlor-6-methyl-anilid) mit n-Bu tylamin reagieren lässt. SUBClaim: Process according to patent claim, characterized in that a ¯-halogen-propionic acid (2-chloro-6-methyl-anilide) is allowed to react with n-butylamine.
CH311632D 1952-02-25 1952-02-25 Process for the production of a new basic substituted fatty acid (2-halogen-6-methyl-anilide). CH311632A (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CH311632T 1952-02-25
CH307799T 1952-11-25

Publications (1)

Publication Number Publication Date
CH311632A true CH311632A (en) 1955-11-30

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CH311632D CH311632A (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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