CH104923A - Process for the production of a thionaphthisatin. - Google Patents

Process for the production of a thionaphthisatin.

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Publication number
CH104923A
CH104923A CH104923DA CH104923A CH 104923 A CH104923 A CH 104923A CH 104923D A CH104923D A CH 104923DA CH 104923 A CH104923 A CH 104923A
Authority
CH
Switzerland
Prior art keywords
thionaphthisatin
chloro
production
condensation
melting point
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 CH104923A publication Critical patent/CH104923A/en

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Description

  

  Verfahren zur Herstellung eines     Thionaphthisatins.       Es wurde gefunden, dass man ein neues       Thionaphthisatin,    das     8-Chlor-1        .2-thionaphth-          isatin,    erhält, wenn man auf     8-Chlor-l-thio-          naphthol,    gegebenenfalls     unter    Zusatz eines       Kondensationsmittels,        Oxalylchlorid    einwir  ken lässt.  



  Das     8-Chlor-1        .2-thionaphthisatin    bildet  ein rotes Pulver, nach einmaligem U     mlösen     aus Benzol erhält man Kristalle vom Schmelz  punkt 238     bis    239  .  



  <I>Beispiel:</I>  194,5 Teile     8-Chlor-l-thion.aphthol        (f rb-          lose    Nadeln vom     Schmelzpunkt    108 bis 109 ")       werden    unter Rühren bei 0   bis<B>10'</B> in etwa.  600 Teile     Oxalyl.chlorid    eingetragen und 20  Stunden bei gewöhnlicher Temperatur ge  rührt.

   Hierauf wird das überschüssige     Oxalyl-          chlorid        abdestilliert    und der     Rückstand,        nach     Zugabe von 1000 Teilen Schwefelkohlenstoff,  unter Rühren     innert    einer Stunde mit 250       Teilen        Aluminium@ehlorid    versetzt, wobei die       Temperatur    bei 0   bis<B>10'</B> gehalten wird.

         Man        rübrt    nun noch längere Zeit bei gewöhn  licher Temperatur, erwärmt     dann    langsam  bis zum Sieden     .des        Schwefelstoffes    und b & -         lässt    eine Stunde bei dieser Temperatur.

   Man       trägt    dann das Reaktionsprodukt in salz  säurehaltiges Wasser     :aus.    Nach dem Abtrei  ben des     Schwefelkohlenstoffes    wird filtriert  und der     Rückstand    mit verdünnter     Sodalösung     bei 50 bis<B>60'</B> ausgezogen; aus der Sofa  lösung wird das     8-Chlor-1        .2-thion.aphthisa-          tin    durch Salzsäure gefällt.



  Process for the production of a thionaphthisatin. It has been found that a new thionaphthisatin, 8-chloro-1 .2-thionaphthisatin, is obtained if oxalyl chloride is allowed to act on 8-chloro-1-thionaphthol, optionally with the addition of a condensing agent.



  The 8-chloro-1,2-thionaphthisatin forms a red powder; after dissolving it once from benzene, crystals with a melting point of 238 to 239 are obtained.



  <I> Example: </I> 194.5 parts of 8-chloro-1-thione.aphthol (colorless needles with a melting point of 108 to 109 ") are mixed with 0 to 10 '' registered in about 600 parts of oxalyl chloride and stirred for 20 hours at ordinary temperature.

   The excess oxalyl chloride is then distilled off and, after the addition of 1000 parts of carbon disulfide, 250 parts of aluminum chloride are added with stirring over the course of one hour, the temperature being kept at 0 to 10 '.

         The mixture is then stirred for a long time at the usual temperature, then slowly warmed to the boiling point of the sulfur and left at this temperature for an hour.

   The reaction product is then carried out in water containing hydrochloric acid: After the carbon disulfide has been stripped off, it is filtered and the residue is extracted with dilute soda solution at 50 to <B> 60 '</B>; 8-chloro-1,2-thione.aphthisatin is precipitated from the sofa solution using hydrochloric acid.

Claims (1)

PATENTANSPRUCH: Verfahren zur Herstellung eines Thio- naphthisatins, des 8-Chlor-1.2-thionaphthisa- tins, dadurch gekennzeichnet, da.ss man auf 8-Chlor-l-thionaphthol Oxa.lylchlorid einwir ken lässt. Das 8-Chlor-1 .2-thionaphthisatin bildet ein rotes Pulver, nach einmaligem Umlösen aus Benzol erhält man Kristalle vom Schmelz punkt 238 bis<B>239'.</B> UNTERANSPRüCHP 1. PATENT CLAIM: A process for the production of a thionaphthisatin, 8-chloro-1,2-thionaphthisatin, characterized in that 8-chloro-1-thionaphthol oxa.lyl chloride is allowed to act. The 8-chloro-1 .2-thionaphthisatin forms a red powder, after redissolving once from benzene crystals with a melting point of 238 to <B> 239 'are obtained. </B> SUBClaim 1. Verfahren nach Patentanspruch, dadurch .gekennzeichnet, da.ss man die Kondensation in Gegenwart eines Kondensationsmittels vornimmt. ?. Verfahren nach Patentanspruch und Un teranspruch 1, dadurch gekennzeichnet, dass Aluminiumchlorid .als Kondensations- mittelgewählt wird. Process according to patent claim, characterized in that the condensation is carried out in the presence of a condensing agent. ?. Method according to patent claim and sub-claim 1, characterized in that aluminum chloride is selected as the condensation agent.
CH104923D 1922-12-02 1922-12-02 Process for the production of a thionaphthisatin. CH104923A (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CH104923T 1922-12-02
CH102033T 1922-12-02

Publications (1)

Publication Number Publication Date
CH104923A true CH104923A (en) 1924-05-16

Family

ID=25706107

Family Applications (1)

Application Number Title Priority Date Filing Date
CH104923D CH104923A (en) 1922-12-02 1922-12-02 Process for the production of a thionaphthisatin.

Country Status (1)

Country Link
CH (1) CH104923A (en)

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