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CH311624A - 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).

Info

Publication number
CH311624A
CH311624A CH311624DA CH311624A CH 311624 A CH311624 A CH 311624A CH 311624D A CH311624D A CH 311624DA CH 311624 A CH311624 A CH 311624A
Authority
CH
Switzerland
Prior art keywords
anilide
methyl
chloro
halogen
propionic acid
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 CH311624A publication Critical patent/CH311624A/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   Verfa. hren zur Herstellmg eines neuen    basisch substituierten Fettsäure- (2-halogen-6  methyl-anilids), welches dadllreh gekennzeieh-    net ist, dass man eine Verbindung der Formel
EMI1.1     
 in weleher X einen reaktionsfähigen, während der Reaktion   sieh      abspaltendenBest    bedeutet, mit   Diäthyla. min    umsetzt.



   Der Rest X kann in einem Halogenatom oder einem sonstigen für den   Austa. usch gegen    den basisehen Rest geeigneten reaktionsfähi  yen    Substit. uenten, wie z. B. einer   Alkylsul-      fonyloxy-oder    Arylsulfonyloxygruppe, bestehen.

   Der Austausch der Gruppe X gegen den Diäthylaminrest erfolgt z.   B.    durch einfaches   Erwärm. en    mit Diäthylamin gegebenenfalls in   Gegenwart eines basisch    reagierenden Konden  sationsmittels    oder von Diäthylami. n im Uber  sehuss.    Das   (3-Diäthyla. mino-propionsäure- (2-    chlor-6-methyl-anilid) ist ein fa. rbloses, auch im Hochvakuum nicht unzersetzt siedendes   i)].    Das Hydrochlorid der Base schmilzt bei   113-114 .   



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



   Beispiel :
31   Gewichtsteile p-Chlor-propionsäure-    (2chlor-6-methyl-anilid) (gewonnen durch Umsetzen von   2-Chlor-6-methyl-a. nilin mit y3-Chlor-    propionsaure-chlorid in Gegenwart von Na  triumacetat, Schmp. 109-112 ) werden    in 80 Gewichtsteilen Äthanol suspendiert und mit 31 Gewichtsteilen Diäthylamin versetzt. Die Temperatur steigt dabei leicht an und ein grosser Teil des   Rea. ktionsgemisches    geht in   Losung.    Nun wird während 4 Stunden bei Zimmertemperatur gerührt und dann einige Stunden bei   65-75 .    Man verdünnt mit Wasser und nimmt das abgeschiedene Öl in Äther auf.

   Nach dem Trocknen der ätherischen Losung und Verjagen des   Losungsmittels    verbleibt ein   öl,    das   durch iYberführen    in das Hydrochlorid gereinigt wird. Man erhält 35 Gewichtsteile reines   p-Diäthylamino-propion-    säure-   (2-chlor-6-methyl-anilid).    Die Umsetzung mit   Diäthyla. min    kann auch in Benzol stattfinden.  



   PATENTANSPRUCH :
Verfahren zur Herstellung eines neuen basisch   substituierten Fettsäure- (2-halogen-6-       methyl-a. nilids), 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).



   Subject of the present patent forms a Verfa. lead to the production of a new, basic substituted fatty acid (2-halogen-6-methyl-anilide), which is marked as a compound of the formula
EMI1.1
 in which X means a reactive best that splits off during the reaction, with diethyla. min implements.



   The radical X can be in a halogen atom or another for the Austa. a suitable reactive substitute against the basic residue. uenten, such as B. an alkylsulfonyloxy or arylsulfonyloxy group exist.

   The exchange of group X against the diethylamine residue takes place z. B. by simple heating. en with diethylamine, optionally in the presence of a basic condensation agent or of diethylamine. n in excess. The (3-diethyla. Mino-propionic acid- (2-chloro-6-methyl-anilide) is a colorless, i) which does not boil undecomposed even in a high vacuum]. The base hydrochloride melts at 113-114.



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



   Example:
31 parts by weight of p-chloro-propionic acid (2-chloro-6-methyl-anilide) (obtained by reacting 2-chloro-6-methyl-a. Niline with y3-chloro-propionic acid chloride in the presence of sodium acetate, melting point 109 -112) are suspended in 80 parts by weight of ethanol and mixed with 31 parts by weight of diethylamine. The temperature rises slightly and a large part of the rea. ction mixture goes into solution. The mixture is then stirred for 4 hours at room temperature and then for a few hours at 65-75. It is diluted with water and the separated oil is taken up in ether.

   After the ethereal solution has dried and the solvent has been driven off, an oil remains which is purified by being converted into the hydrochloride. 35 parts by weight of pure p-diethylamino-propionic acid (2-chloro-6-methyl-anilide) are obtained. Implementation with Diethyla. min can also take place in benzene.



   PATENT CLAIM:
Process for the preparation of a new, basic substituted fatty acid (2-halogen-6-methyl-a. Nilids), 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 Verfa. hren zur Herstellmg eines neuen basisch substituierten Fettsäure- (2-halogen-6 methyl-anilids), welches dadllreh gekennzeieh- net ist, dass man eine Verbindung der Formel EMI1.1 in weleher X einen reaktionsfähigen, während der Reaktion sieh abspaltendenBest bedeutet, mit Diäthyla. min umsetzt. Subject of the present patent forms a Verfa. lead to the production of a new, basic substituted fatty acid (2-halogen-6-methyl-anilide), which is marked as a compound of the formula EMI1.1 in which X means a reactive best that splits off during the reaction, with diethyla. min implements. Der Rest X kann in einem Halogenatom oder einem sonstigen für den Austa. usch gegen den basisehen Rest geeigneten reaktionsfähi yen Substit. uenten, wie z. B. einer Alkylsul- fonyloxy-oder Arylsulfonyloxygruppe, bestehen. The radical X can be in a halogen atom or another for the Austa. a suitable reactive substitute against the basic residue. uenten, such as B. an alkylsulfonyloxy or arylsulfonyloxy group exist. Der Austausch der Gruppe X gegen den Diäthylaminrest erfolgt z. B. durch einfaches Erwärm. en mit Diäthylamin gegebenenfalls in Gegenwart eines basisch reagierenden Konden sationsmittels oder von Diäthylami. n im Uber sehuss. Das (3-Diäthyla. mino-propionsäure- (2- chlor-6-methyl-anilid) ist ein fa. rbloses, auch im Hochvakuum nicht unzersetzt siedendes i)]. Das Hydrochlorid der Base schmilzt bei 113-114 . The exchange of group X against the diethylamine residue takes place z. B. by simple heating. en with diethylamine, optionally in the presence of a basic condensation agent or of diethylamine. n in excess. The (3-diethyla. Mino-propionic acid- (2-chloro-6-methyl-anilide) is a colorless, i) which does not boil undecomposed even in a high vacuum]. The base hydrochloride melts at 113-114. Das neue Anilid soll als Lokalanästhetikum und als Zwischenprodukt zur Herstellung weiterer Derivate Verwendung finden. The new anilide is to be used as a local anesthetic and as an intermediate product for the production of further derivatives. Beispiel : 31 Gewichtsteile p-Chlor-propionsäure- (2chlor-6-methyl-anilid) (gewonnen durch Umsetzen von 2-Chlor-6-methyl-a. nilin mit y3-Chlor- propionsaure-chlorid in Gegenwart von Na triumacetat, Schmp. 109-112 ) werden in 80 Gewichtsteilen Äthanol suspendiert und mit 31 Gewichtsteilen Diäthylamin versetzt. Die Temperatur steigt dabei leicht an und ein grosser Teil des Rea. ktionsgemisches geht in Losung. Nun wird während 4 Stunden bei Zimmertemperatur gerührt und dann einige Stunden bei 65-75 . Man verdünnt mit Wasser und nimmt das abgeschiedene Öl in Äther auf. Example: 31 parts by weight of p-chloro-propionic acid (2-chloro-6-methyl-anilide) (obtained by reacting 2-chloro-6-methyl-a. Niline with y3-chloro-propionic acid chloride in the presence of sodium acetate, melting point 109 -112) are suspended in 80 parts by weight of ethanol and mixed with 31 parts by weight of diethylamine. The temperature rises slightly and a large part of the rea. ction mixture goes into solution. The mixture is then stirred for 4 hours at room temperature and then for a few hours at 65-75. It is diluted with water and the separated oil is taken up in ether. Nach dem Trocknen der ätherischen Losung und Verjagen des Losungsmittels verbleibt ein öl, das durch iYberführen in das Hydrochlorid gereinigt wird. Man erhält 35 Gewichtsteile reines p-Diäthylamino-propion- säure- (2-chlor-6-methyl-anilid). Die Umsetzung mit Diäthyla. min kann auch in Benzol stattfinden. After the ethereal solution has dried and the solvent has been driven off, an oil remains which is purified by being converted into the hydrochloride. 35 parts by weight of pure p-diethylamino-propionic acid (2-chloro-6-methyl-anilide) are obtained. Implementation with Diethyla. min can also take place in benzene. PATENTANSPRUCH : Verfahren zur Herstellung eines neuen basisch substituierten Fettsäure- (2-halogen-6- methyl-a. nilids), dadurch gekennzeichnet, dass man eine Verbindung der Formel EMI1.2 in welcher X einen reaktionsfähigen, während der Reaktion sich abspaltenden Rest bedeutet, mit Diäthylamin umsetzt. Das auf diese Weise erhaltene @-Diäthylamino-propionsäure- (2- ehlor-6-met. hyl-anilid) bildet ein farbloses, auch im Hochvakuum nicht unzersetzt sieden d, es 61. Das Hydrochlorid der Base schmilzt bei 113 - 114 Das neue Anilid soll als Lokalanästhetikum und als Zwisehenprodukt Verwendung finden. PATENT CLAIM: Process for the preparation of a new, basic substituted fatty acid (2-halogen-6-methyl-a. Nilids), characterized in that a compound of the formula EMI1.2 in which X is a reactive radical which is split off during the reaction, is reacted with diethylamine. The @ -diethylamino-propionic acid- (2-chloro-6-meth. Hyl-anilide) obtained in this way forms a colorless, which does not boil undecomposed even in a high vacuum The new anilide is to be used as a local anesthetic and as an intermediate product. UNTERANSPRUCH : Verfahren nach Patentanspruch, dadurch gekennzeichnet, dass man ein p-Halogen-pro pionsäure- (2-ehlor-6-methyl-anilid) mit Di äthyla. min reagieren lässt. SUBClaim: Process according to patent claim, characterized in that a p-halogen-propionic acid (2-chloro-6-methyl-anilide) with diethyla. min reacts.
CH311624D 1952-02-25 1952-02-25 Process for the production of a new basic substituted fatty acid (2-halogen-6-methyl-anilide). CH311624A (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CH311624T 1952-02-25
CH307799T 1952-11-25

Publications (1)

Publication Number Publication Date
CH311624A true CH311624A (en) 1955-11-30

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Family Applications (1)

Application Number Title Priority Date Filing Date
CH311624D CH311624A (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) CH311624A (en)

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