CH311645A - Process for the production of a new basic substituted fatty acid amide. - Google Patents

Process for the production of a new basic substituted fatty acid amide.

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Publication number
CH311645A
CH311645A CH311645DA CH311645A CH 311645 A CH311645 A CH 311645A CH 311645D A CH311645D A CH 311645DA CH 311645 A CH311645 A CH 311645A
Authority
CH
Switzerland
Prior art keywords
diethylamine
phenoxy
amide
acid
fatty 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 CH311645A publication Critical patent/CH311645A/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 FettsÏureamides.



   Gegenstand des vorliegenden Patentes bildet ein Verfahren zur Herstellung eines neuen basisch substituierten Fettsäureamides, welehes dadurch gekennzeichnet ist, dass man eine Verbindung der Formel
EMI1.1     
 in   welcher X    einen   reaktionsfähigen, wäh-    rend der Reaktion sich abspaltenden Rest bedeutet, mit Diäthylamin 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   Alkylsulfonyl-    oxy-oder Arylsulfonyloxygruppe, bestehen.



  Der Austausch der Gruppe   X    gegen den Di  athylaminorest    erfolgt z. B. durch einfaches Erwärmen mit Diäthylamin gegebenenfalls in Gegenwart eines basisch reagierenden   Kon-    densationsmittels oder von Diäthylamin im Überschuss. Das Diäthylaminoessigsäure-N-(2  phenoxy-äthyl-1)-methyl-amid    ist ein farbloses, unter 0, 02 mm bei 136-137  siedendes   61.   



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



   Beispiel :    22,    7 g ChloressigsÏure-N-(2-phenoxy-Ïthyl1)-methylamid und 16, 1g Diäthylamin werden zusammen in 200   cm3    abs. Benzol 4 Stunden auf dem Wasserbad erhitzt. Das Reak  tionsgemisch    wird mit Wasser ausgeschüttelt und dann mit 2n-Salzsäure ausgezogen. Darauf 'wird der salzsaure Auszug mit Äther extrahiert, unter Eiskühlung mit konz. Natronlauge versetzt und das ausgeschiedene öl in Äther aufgenommen. Nach dem Trocknen   der Ätherauszüge über Pottasche    wird der Äther verdampft und der Rückstand im Hochvakuum destilliert.



   Dabei gewinnt man das unter 0, 02 mm bei   136-137     siedende Diäthylaminoessigsäure-N- (2-phenoxy-äthyl-1)-methylamid in einer Ausbeute von 72, 2% der Theorie. Farbloses   öl,    schwer löslich in Wasser, gut in organischen Lösungsmitteln und in   verdünn-    ten Mineralsäuren.  



   PATENTANSPRUCH :
Verfahren zur Herstellung eines neuen basisch substituierten Fettsäureamides, dadurch gekennzeichnet, dass man eine Verbindung der Formel
EMI1.2     
 in welcher X einen reaktionsfähigen, während der Reaktion sich abspaltenden Rest   bedeu-    tet, mit Diäthylamin umsetzt. Das auf diese Weise erhaltene   Diäthylaminoessigsäure-N- (2-      phenoxy-äthyl-1)-methylamid    bildet ein farbloses, unter 0, 02 mm bei 136-137  siedendes Íl. 

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





  



  Process for the production of a new basic substituted fatty acid amide.



   The subject of the present patent forms a process for the preparation of a new basic substituted fatty acid amide, 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, is reacted with diethylamine.



   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 alkylsulfonyl oxy or arylsulfonyloxy group exist.



  The exchange of group X against the diethylamino radical takes place, for. B. by simply heating with diethylamine, optionally in the presence of a basic condensing agent or diethylamine in excess. Diethylaminoacetic acid-N- (2-phenoxy-ethyl-1) -methyl-amide is a colorless 61, boiling below 0.02 mm at 136-137.



  The new amide will be used as a local anesthetic and as an intermediate for the production of other derivatives.



   Example: 22.7 g of chloroacetic acid-N- (2-phenoxy-Ïthyl1) -methylamide and 16.1g of diethylamine are combined in 200 cm3 of abs. Benzene heated on a water bath for 4 hours. The reaction mixture is extracted with water and then extracted with 2N hydrochloric acid. The hydrochloric acid extract is then extracted with ether, with ice cooling with conc. Sodium hydroxide solution was added and the oil which had separated out was taken up in ether. After the ether extracts have been dried over potash, the ether is evaporated and the residue is distilled in a high vacuum.



   The diethylaminoacetic acid-N- (2-phenoxy-ethyl-1) -methylamide boiling below 0.02 mm at 136-137 is obtained in a yield of 72.2% of theory. Colorless oil, sparingly soluble in water, good in organic solvents and in dilute mineral acids.



   PATENT CLAIM:
Process for the preparation of a new basic substituted fatty acid amide, characterized in that a compound of the formula
EMI1.2
 in which X means a reactive residue that is split off during the reaction, reacts with diethylamine. The diethylaminoacetic acid-N- (2-phenoxy-ethyl-1) -methylamide obtained in this way forms a colorless oil which boils below 0.02 mm at 136-137.

** 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 FettsÏureamides. Process for the production of a new basic substituted fatty acid amide. Gegenstand des vorliegenden Patentes bildet ein Verfahren zur Herstellung eines neuen basisch substituierten Fettsäureamides, welehes dadurch gekennzeichnet ist, dass man eine Verbindung der Formel EMI1.1 in welcher X einen reaktionsfähigen, wäh- rend der Reaktion sich abspaltenden Rest bedeutet, mit Diäthylamin umsetzt. The subject of the present patent forms a process for the preparation of a new basic substituted fatty acid amide, 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, is reacted with diethylamine. Der Rest X kann in einem Halogenatom oder einem sonstigen für den Austausch gegen den basischen Rest geeigneten reaktionsfähigen Substituenten, wie z. B. einer Alkylsulfonyl- oxy-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 alkylsulfonyl oxy or arylsulfonyloxy group exist. Der Austausch der Gruppe X gegen den Di athylaminorest erfolgt z. B. durch einfaches Erwärmen mit Diäthylamin gegebenenfalls in Gegenwart eines basisch reagierenden Kon- densationsmittels oder von Diäthylamin im Überschuss. Das Diäthylaminoessigsäure-N-(2 phenoxy-äthyl-1)-methyl-amid ist ein farbloses, unter 0, 02 mm bei 136-137 siedendes 61. The exchange of group X against the diethylamino radical takes place, for. B. by simply heating with diethylamine, optionally in the presence of a basic condensing agent or diethylamine in excess. Diethylaminoacetic acid-N- (2-phenoxy-ethyl-1) -methyl-amide is a colorless 61, boiling below 0.02 mm at 136-137. Das neue Amid soll als Lokalanästhetikum und als Zwischenprodukt zur Herstellung weiterer Derivate Verwendung finden. The new amide will be used as a local anesthetic and as an intermediate for the production of other derivatives. Beispiel : 22, 7 g ChloressigsÏure-N-(2-phenoxy-Ïthyl1)-methylamid und 16, 1g Diäthylamin werden zusammen in 200 cm3 abs. Benzol 4 Stunden auf dem Wasserbad erhitzt. Das Reak tionsgemisch wird mit Wasser ausgeschüttelt und dann mit 2n-Salzsäure ausgezogen. Darauf 'wird der salzsaure Auszug mit Äther extrahiert, unter Eiskühlung mit konz. Natronlauge versetzt und das ausgeschiedene öl in Äther aufgenommen. Nach dem Trocknen der Ätherauszüge über Pottasche wird der Äther verdampft und der Rückstand im Hochvakuum destilliert. Example: 22.7 g of chloroacetic acid-N- (2-phenoxy-Ïthyl1) -methylamide and 16.1g of diethylamine are combined in 200 cm3 of abs. Benzene heated on a water bath for 4 hours. The reaction mixture is extracted with water and then extracted with 2N hydrochloric acid. The hydrochloric acid extract is then extracted with ether, with ice cooling with conc. Sodium hydroxide solution was added and the oil which had separated out was taken up in ether. After the ether extracts have been dried over potash, the ether is evaporated and the residue is distilled in a high vacuum. Dabei gewinnt man das unter 0, 02 mm bei 136-137 siedende Diäthylaminoessigsäure-N- (2-phenoxy-äthyl-1)-methylamid in einer Ausbeute von 72, 2% der Theorie. Farbloses öl, schwer löslich in Wasser, gut in organischen Lösungsmitteln und in verdünn- ten Mineralsäuren. The diethylaminoacetic acid-N- (2-phenoxy-ethyl-1) -methylamide boiling below 0.02 mm at 136-137 is obtained in a yield of 72.2% of theory. Colorless oil, sparingly soluble in water, good in organic solvents and in dilute mineral acids. PATENTANSPRUCH : Verfahren zur Herstellung eines neuen basisch substituierten Fettsäureamides, dadurch gekennzeichnet, dass man eine Verbindung der Formel EMI1.2 in welcher X einen reaktionsfähigen, während der Reaktion sich abspaltenden Rest bedeu- tet, mit Diäthylamin umsetzt. Das auf diese Weise erhaltene Diäthylaminoessigsäure-N- (2- phenoxy-äthyl-1)-methylamid bildet ein farbloses, unter 0, 02 mm bei 136-137 siedendes Íl. PATENT CLAIM: Process for the preparation of a new basic substituted fatty acid amide, characterized in that a compound of the formula EMI1.2 in which X means a reactive residue that is split off during the reaction, reacts with diethylamine. The diethylaminoacetic acid-N- (2-phenoxy-ethyl-1) -methylamide obtained in this way forms a colorless oil which boils below 0.02 mm at 136-137. Das neue Amid soll als Lokalanästhetikum und als Zwischenprodukt Verwendung finden. The new amide will be used as a local anesthetic and as an intermediate product. UNTERANSPRUCH : Verfahren nach Patentanspruch, dadurch gekennzeiehhet, dass man ein Halogenessig- säure-N- (2-phenoxy-Ïthyl-1)-methylamid mit Diäthylamin reagieren lϯl. SUBClaim: Process according to claim, characterized in that a haloacetic acid-N- (2-phenoxy--thyl-1) -methylamide is reacted with diethylamine.
CH311645D 1952-06-08 1952-06-08 Process for the production of a new basic substituted fatty acid amide. CH311645A (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CH311645T 1952-06-08
CH307799T 1952-11-25

Publications (1)

Publication Number Publication Date
CH311645A true CH311645A (en) 1955-11-30

Family

ID=25735378

Family Applications (1)

Application Number Title Priority Date Filing Date
CH311645D CH311645A (en) 1952-06-08 1952-06-08 Process for the production of a new basic substituted fatty acid amide.

Country Status (1)

Country Link
CH (1) CH311645A (en)

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