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DE819401C - Process for the preparation of bis-cyanoalkylanilines - Google Patents

Process for the preparation of bis-cyanoalkylanilines

Info

Publication number
DE819401C
DE819401C DEP52447A DEP0052447A DE819401C DE 819401 C DE819401 C DE 819401C DE P52447 A DEP52447 A DE P52447A DE P0052447 A DEP0052447 A DE P0052447A DE 819401 C DE819401 C DE 819401C
Authority
DE
Germany
Prior art keywords
bis
preparation
cyanoalkylanilines
acrylonitrile
weight
Prior art date
Legal status (The legal status 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 status listed.)
Expired
Application number
DEP52447A
Other languages
German (de)
Inventor
Walter Dr Franke
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Huels AG
Original Assignee
Chemische Werke Huels 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 Chemische Werke Huels AG filed Critical Chemische Werke Huels AG
Priority to DEP52447A priority Critical patent/DE819401C/en
Application granted granted Critical
Publication of DE819401C publication Critical patent/DE819401C/en
Expired legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C255/00Carboxylic acid nitriles

Landscapes

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

Description

Verfahren zur Herstellung von Bis-cyanalkylanilinen Man hat schon a, ß-ungesättigte Nitrile mit Aminen kondensiert, wobei die aromatischen Amine wesentlich schwerer als die aliphatischen Amine mit den a, ß-ungesättigten Nitrilen, z.,B. Acrylnitril, reagieren. Während Anilin in Gegenwart von alkalischen oder sauren Mitteln Acrylnitril noch anlagert, reagiert z. B. Monomethylanilin mit Acrylnitril auch in Gegenwart sehr wirksamer Katalysatoren selbst bei r8o° nicht.Process for the preparation of bis-cyanoalkylanilines One already has a, ß-unsaturated nitriles condensed with amines, the aromatic amines being essential heavier than the aliphatic amines with the α, ß-unsaturated nitriles, e.g. Acrylonitrile, react. While aniline in the presence of alkaline or acidic Means acrylonitrile still attaches, z. B. monomethylaniline with acrylonitrile not even in the presence of very effective catalysts, even at r80 °.

Es wurde nun gefunden, daB man wertvolle Kondensationsprodukte erhalten kann, wenn .man N-Cyanmethvlaniline mit Acrylnitril in Gegenwart alkalisch wirkender -Mittel umsetzt. Die N-Cyanmethvlaniline sind leicht aus Anilin oder dessen Kernsubstitutionsprodukten, Blausäure und Formaldehyd, erhältlich. Als alkalisch wirkende Mittel kommen insbesondere die Alkalialkoholate in Betracht, doch kann man auch mit Alkalilaugen oder Aminen, wie Piperidin, Trimethylbenzylammoniumhydroxyd usw., arbeiten. Man nimmt zweckmäßig die Umsetzung in Gegenwart von Lösungsmitteln oder Verdünnungsmitteln vor.It has now been found that valuable condensation products are obtained can, if .man N-Cyanmethvlaniline with acrylonitrile in the presence of alkaline acting -Means implement. The N-Cyanmethvlaniline are easily made from aniline or its core substitution products, Hydrocyanic acid and formaldehyde, available. As alkaline agents come in particular the alkali alcoholates into consideration, but one can also use alkali lye or amines, such as piperidine, trimethylbenzylammonium hydroxide, etc., work. One takes appropriately the reaction in the presence of solvents or diluents before.

Die erhaltenen N-Cyanmethyl-N-cyanäthylaniline können als Zwischenprodukte für die Herstellung von Farbstoffen, Textilhilfsmitteln usw. Verwenc'.ung finden.The N-cyanomethyl-N-cyanoethylanilines obtained can be used as intermediates for the production of dyes, textile auxiliaries, etc. use.

Beispiel Man legt ein Gemisch aus 5o Gewichtsteilen Dioxan und r Gewichtsteil festem Natriumäthylat vor und trägt sodann bei 30° ein Gemisch aus 26 Gewichtsteilen N-Cyanmethylaniliii und .45 Gewichtsteilen Acrylnitril allmählich ein, rührt nach beendetem Eintragen noch einige Zeit bei 30° nach, neutralisiert mit Essigsäure und destilliert Dioxan und überschüssiges Acrylnitril ab. Der dunkelbraune, dickflüssige Rückstand wird mit Benzol ausgekocht, wobei sich das Reaktionsprodukt löst, während harzige Schmieren ungelöst bleiben. Man trennt die Benzollösung vom Rückstand ab, destilliert das Benzol ab und erhält beim Kp2 mm 2o5° als hellgelbe Kristalle N-Cyanmethyl-N-cyanäthylanilin vom Schmelzpunkt 52 bis 62°. Nach dem Umlösen aus Methanol steigt der Schmelzpunkt auf 67 bis 68°, Ausbeute 22 Gewichtsteile = 6o% der Theorie. In analoger Weise arbeitet man bei Verwendung von kernsubstituierten N-C@: anmeth@-lanilincn. Die Umsetzung gelingt auch in Toluol, jedoch bei wesentlich längeren Reaktionszeiten. EXAMPLE A mixture of 50 parts by weight of dioxane and r part by weight of solid sodium ethylate is initially introduced and a mixture of 26 parts by weight of N-cyanomethylaniliii and 45 parts by weight of acrylonitrile is then gradually introduced at 30 °, and after the addition is complete, the mixture is stirred for a while at 30 °, neutralized with acetic acid and distilled off dioxane and excess acrylonitrile. The dark brown, viscous residue is boiled with benzene, the reaction product dissolving while resinous smear remains undissolved. The benzene solution is separated off from the residue, the benzene is distilled off and at a bp 2 mm 2o5 °, pale yellow crystals of N-cyanomethyl-N-cyanoethylaniline with a melting point of 52 to 62 ° are obtained. After this Dissolving from methanol, the melting point rises 67 to 68 °, yield 22 parts by weight = 6o% of the Theory. You work in an analogous way when using of core-substituted NC @: anmeth @ -lanilincn. The reaction also works in toluene, however with significantly longer response times.

Claims (1)

PATENTANSPRUCH: Verfahren zur Herstellung N-on Bis-cyanalkyl- anilinen, dadurch gekennzeichnet, daB man N-Cyanmethylaniliii° mit :\cr@-liiitril -in Geg°n- wart alkalisch wirkender Mittel umsetzt.
PATENT CLAIM: Process for the preparation of N-one bis-cyanoalkyl anilines, characterized in that one N-Cyanmethylaniliii ° with: \ cr @ -liiitril -in Geg ° n- was using alkaline agents.
DEP52447A 1949-08-20 1949-08-20 Process for the preparation of bis-cyanoalkylanilines Expired DE819401C (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
DEP52447A DE819401C (en) 1949-08-20 1949-08-20 Process for the preparation of bis-cyanoalkylanilines

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DEP52447A DE819401C (en) 1949-08-20 1949-08-20 Process for the preparation of bis-cyanoalkylanilines

Publications (1)

Publication Number Publication Date
DE819401C true DE819401C (en) 1951-10-31

Family

ID=7385757

Family Applications (1)

Application Number Title Priority Date Filing Date
DEP52447A Expired DE819401C (en) 1949-08-20 1949-08-20 Process for the preparation of bis-cyanoalkylanilines

Country Status (1)

Country Link
DE (1) DE819401C (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2809985A (en) * 1956-04-10 1957-10-15 Gen Aniline & Film Corp Bis-cyanoethylated anilines

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2809985A (en) * 1956-04-10 1957-10-15 Gen Aniline & Film Corp Bis-cyanoethylated anilines

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