CH314560A - Process for the preparation of di- (m, p'-guanidino) -diazoaminobenzene dihydrochloride - Google Patents

Process for the preparation of di- (m, p'-guanidino) -diazoaminobenzene dihydrochloride

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Publication number
CH314560A
CH314560A CH314560DA CH314560A CH 314560 A CH314560 A CH 314560A CH 314560D A CH314560D A CH 314560DA CH 314560 A CH314560 A CH 314560A
Authority
CH
Switzerland
Prior art keywords
guanidino
dihydrochloride
diazoaminobenzene
preparation
solution
Prior art date
Application number
Other languages
German (de)
Inventor
Heinrich Dr Jensch
Original Assignee
Hoechst 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 Hoechst Ag filed Critical Hoechst Ag
Publication of CH314560A publication Critical patent/CH314560A/en

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Description

  

  Verfahren zur Herstellung von     Di-(m,p'-guanidino)-diazoaminobenzol-dihydrochlorid       Das Verfahrensprodukt stellt ein gelbliches  Pulver dar, das nach     Umkristallisieren    aus  Methanol und Aceton bei 185      -unter    Zerset  zung schmilzt. Es zeichnet sich durch hervor  ragende     Wirksamkeit    gegen Blutparasiten,  z. B.     Trvpanosomen,        Babesien    u. a., aus.

      <I>Beispiel</I>         Gegenstand    des vorliegenden Zusatzpaten  tes ist ein Verfahren zur Herstellung von     Di-          (m,p'-guanidino)    -     diazoaminoben7ol-dihydro-          ehlorid,    das dadurch gekennzeichnet ist, dass  man     m-Guanidino-phenyldiazoniumchlorid    in       sehwach    saurer Lösung mit     p-Amino-phenyl-          guanidin-hyclrochlorid    umsetzt.

    
EMI0001.0016     
    25 g     m-Acetamino-phenylguanidincarbonat     (F. 118 ) werden durch einstündiges Erwär  men mit 160     ein-    Wasser und 40     cm3    konzen  trierter Salzsäure im Wasserbad verseift. Die  erhaltene Lösung des     salzsauren        m-Amino-          phenylguanidins    wird mit 7 g     Natriumnitrit     dianotiert und mit einer Lösung von salzsau  rem     p-Amino-phenylguanidin    aus 25 g     p-Acet-          amino-phenylguanidin-carbonat    vermischt.

    Auf Zusatz von überschüssiger     gesättigter    Na  triumchloridlösung und etwa     1.00        em3    gesät  tigter     Natriumacetatlösung    zu der eiskalten  Mischung bildet sieh ein lehmgelber Brei, der         naeh    einiger Zeit abgesaugt und mit verdünn  ter     Kochsalzlösung,    wenig eiskaltem Wasser  und Aceton gewaschen     wird.    Nach dem Um  kristallisieren aus Methanol und Aceton erhält  man ein gelbes Pulver, das das     Dihydrochlo-          rid    des     Di-(m,p'-gtianidino)-diazoaminobenzols     darstellt. F. 185  unter Zersetzung. Es ist  leicht löslich in Wasser.  



  Durch Behandeln mit     Sodalösung    erhält  man ein harzartiges     Carbonat,    das beim Rei  ben fest     wird    und,     aus    Wasser umkristalli  siert, ein graugelbes Pulver vom F. 149-150   unter langsamer Zersetzung darstellt.



  Process for the preparation of di- (m, p'-guanidino) diazoaminobenzene dihydrochloride The process product is a yellowish powder which, after recrystallization from methanol and acetone at 185 °, melts with decomposition. It is characterized by its excellent effectiveness against blood parasites, e.g. B. Trvpanosomes, Babesia u. a., off.

      <I> Example </I> The subject matter of the present additional patent is a process for the preparation of di- (m, p'-guanidino) - diazoaminoben7ol-dihydrochloride, which is characterized in that m-guanidino-phenyldiazonium chloride is used in a very weak state acidic solution with p-amino-phenyl-guanidine-hydrochloride.

    
EMI0001.0016
    25 g of m-acetaminophenylguanidine carbonate (F. 118) are saponified by heating for one hour with 160 one-piece water and 40 cm3 of concentrated hydrochloric acid in a water bath. The resulting solution of hydrochloric acid m-aminophenylguanidine is dianotized with 7 g of sodium nitrite and mixed with a solution of hydrochloric acid rem p-aminophenylguanidine from 25 g of p-acetaminophenylguanidine carbonate.

    When excess saturated sodium chloride solution and about 1.00 em3 saturated sodium acetate solution are added to the ice-cold mixture, a clay-yellow pulp is formed, which is sucked off after a while and washed with dilute sodium chloride solution, a little ice-cold water and acetone. After recrystallization from methanol and acetone, a yellow powder is obtained which is the dihydrochloride of di- (m, p'-gtianidino) -diazoaminobenzene. F. 185 with decomposition. It is easily soluble in water.



  By treating with soda solution, a resinous carbonate is obtained, which solidifies on Rei ben and, recrystallized from water, is a gray-yellow powder of F. 149-150 with slow decomposition.

 

Claims (1)

PATENTANSPRUCH Verfahren zur Herstelhmg von Di-(m,p'- guanidino) - diazoaminobenzol - dihy drochlorid, dadurch gekennzeichnet, dass man m-Guani- dino-phenyldiazoniumchlorid in schwach sau rer Lösung mit p-Amino-phenyjgnanidin-hy- drochlorid umsetzt. Das Verfahrensprodukt stellt ein gelbes Pulver dar, das nach L mkristallisieren aus Methanol und Aceton bei 185 unter Zerset zung schmilzt. PATENT CLAIM A process for the production of di- (m, p'-guanidino) - diazoaminobenzene - dihydrochloride, characterized in that m-guanidino-phenyldiazonium chloride is reacted in weakly acidic solution with p-aminophenyjgnanidine hydrochloride. The product of the process is a yellow powder which, after crystallizing from methanol and acetone, melts at 185 ° C. with decomposition.
CH314560D 1951-05-21 1952-05-19 Process for the preparation of di- (m, p'-guanidino) -diazoaminobenzene dihydrochloride CH314560A (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE314560X 1951-05-21
CH306506T 1952-05-19

Publications (1)

Publication Number Publication Date
CH314560A true CH314560A (en) 1956-06-15

Family

ID=25735169

Family Applications (1)

Application Number Title Priority Date Filing Date
CH314560D CH314560A (en) 1951-05-21 1952-05-19 Process for the preparation of di- (m, p'-guanidino) -diazoaminobenzene dihydrochloride

Country Status (1)

Country Link
CH (1) CH314560A (en)

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