CH104927A - Process for the production of a thionaphthisatin. - Google Patents

Process for the production of a thionaphthisatin.

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Publication number
CH104927A
CH104927A CH104927DA CH104927A CH 104927 A CH104927 A CH 104927A CH 104927D A CH104927D A CH 104927DA CH 104927 A CH104927 A CH 104927A
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CH
Switzerland
Prior art keywords
thionaphthisatin
bromo
production
condensation
chloride
Prior art date
Application number
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German (de)
Inventor
Gesellschaft Fuer Chemis Basel
Original Assignee
Chem Ind Basel
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 Chem Ind Basel filed Critical Chem Ind Basel
Publication of CH104927A publication Critical patent/CH104927A/en

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Description

       

  Verfahren zur Herstellung eines     Thionaphthisatins.       Es wurde gefunden, dass man ein neues       Thionaphthisatin,    das     5-Brom-2.        1-thionaphth-          isatin    erhält, wenn man auf     5-Brom-2-thio-          naphthol        Oxalylchlorid,    gegebenenfalls unter  Zusatz eines Kondensationsmittels, einwirken  lässt.  



  Das     5-Brom-2        .1-thionaphthisatin    bildet  ein rotes Pulver, nach einmaligem     Umlösen     aus Benzol erhält man Kristalle vom     Sp.    212  bis 213  .  



  <I>Beispiel:</I>  239 Teile     5-Brom-2-thionaphthol    (farblose  Nadeln vom     Sp.    50-51  ) werden unter Rüh  ren bei 0   bis 10   in etwa 600 Teile     Oxalyl-          chlorid    eingetragen und 20 Stunden bei ge  wöhnlicher Temperatur gerührt. Hierauf wird  das überschüssige     Oxalylchlorid        abdestilliert     und der Rückstand, nach Zugabe von     1_000     Teilen     Schwefelkohlenstoff,    unter Rühren     in-          nert    einer Stunde mit 250 Teilen Aluminium  chlorid versetzt, wobei die Temperatur bei 0   bis 10   gehalten wird.

   Man rührt nun noch  längere Zeit bei gewöhnlicher Temperatur,    erwärmt dann langsam bis zum Sieden des       Schwefelkohlenstoffes    und belässt 1 Stunde  bei dieser Temperatur. Man trägt dann das  Reaktionsprodukt in salzsäurehaltiges Wasser  aus. Nach dem Abtreiben des     Schwefelkohlen-          stoffes    wird filtriert und der Rückstand mit  verdünnter     Sodalösung    bei 50-60   ausge  zogen; aus der     Sodalösung    wird das     5-Brotn-          2    .     1-thionaphthisatin    durch Salzsäure gefällt.



  Process for the production of a thionaphthisatin. It has been found that a new thionaphthisatin, 5-bromo-2. 1-thionaphthisatin is obtained when oxalyl chloride is allowed to act on 5-bromo-2-thionaphthol, optionally with the addition of a condensing agent.



  The 5-bromo-2 .1-thionaphthisatin forms a red powder, after dissolving once from benzene crystals from col. 212 to 213 are obtained.



  <I> Example: </I> 239 parts of 5-bromo-2-thionaphthol (colorless needles from Sp. 50-51) are added to about 600 parts of oxalyl chloride with stirring at 0 to 10 and for 20 hours at normal Temperature stirred. The excess oxalyl chloride is then distilled off and, after the addition of 1,000 parts of carbon disulfide, 250 parts of aluminum chloride are added with stirring within one hour, the temperature being kept at 0-10.

   The mixture is then stirred for a longer time at the usual temperature, then heated slowly until the carbon disulfide boils and left at this temperature for 1 hour. The reaction product is then discharged into water containing hydrochloric acid. After the carbon disulfide has been driven off, it is filtered and the residue is extracted with dilute soda solution at 50-60; the soda solution becomes the 5-bread 2. 1-thionaphthisatin precipitated by hydrochloric acid.

Claims (1)

PATENTANSPRUCH: Verfahren zur Herstellung eines Thio- naphthisatins, des 5-Brom-2 .1-thionaphth- isatins, dadurch gekennzeichnet, dass man auf 5-Brom-2-thionaphthol Oxalylahlorid ein wirken lässt. Das 5-Brom-2 .1-thionaphthisatin bildet ein rotes Pulver, nach einmaligem Umlösen aus Benzol erhält man Kristalle vom Sp. 212 bis 213 . UNTERANSPRÜUCHE-: 1. PATENT CLAIM: Process for the production of a thionaphthisatin, 5-bromo-2 .1-thionaphthisatin, characterized in that oxalyla chloride is allowed to act on 5-bromo-2-thionaphthol. The 5-bromo-2 .1-thionaphthisatin forms a red powder, after dissolving once from benzene crystals from col. 212 to 213 are obtained. SUBClaims-: 1. Verfahren nach Patentanspruch, dadurch gekennzeichnet, dass man die Kondensation in Gegenwart eines Kondensationsmittels vornimmt. 2. Verfahren nach Patentanspruch und Unter anspruch 1, dadurch gekennzeichnet, dass Aluminiumchlorid als Kondensationsmittel gewählt wird. Process according to claim, characterized in that the condensation is carried out in the presence of a condensing agent. 2. The method according to claim and sub-claim 1, characterized in that aluminum chloride is selected as the condensation agent.
CH104927D 1922-12-02 1922-12-02 Process for the production of a thionaphthisatin. CH104927A (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CH104927T 1922-12-02
CH102033T 1922-12-02

Publications (1)

Publication Number Publication Date
CH104927A true CH104927A (en) 1924-05-16

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Family Applications (1)

Application Number Title Priority Date Filing Date
CH104927D CH104927A (en) 1922-12-02 1922-12-02 Process for the production of a thionaphthisatin.

Country Status (1)

Country Link
CH (1) CH104927A (en)

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