CH104924A - Process for the production of a thionaphthisatin. - Google Patents
Process for the production of a thionaphthisatin.Info
- Publication number
- CH104924A CH104924A CH104924DA CH104924A CH 104924 A CH104924 A CH 104924A CH 104924D A CH104924D A CH 104924DA CH 104924 A CH104924 A CH 104924A
- Authority
- CH
- Switzerland
- Prior art keywords
- chloro
- thionaphthisatin
- production
- condensation
- oxalyl chloride
- Prior art date
Links
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Description
Verfahren zur Herstellung eines Thionaphthisatins. Es wurde ,gefunden, @dass man ein neues Thionaphthisatin, das 1-Chlor-2.3-thionaphth- isatin, erhält, wenn man auf 1-Chlor-2-thio- napUthol Oxalylchlorid, gegebenenfalls unter Zusatz eines Kondensationsmittels, einwir- ken lässt.
Das 1-Chlor-2 .3-thionaphthisatin bildet ein rotes Pulver, nach einmaligem Umlösen aus Benzol erhält man Kristalle vom Schmelz punkt 194'.
Beispiel: 194,5 Teile 1-Chlor-2-thiona,-phtliol (farb lose Nadeln vom Schmelzpunkt 51 ) werden unter Rühren bei 0 bis 10 in etwa 600 Teile Oxalylchlorid eingetragen und 20 Stunden bei gewöhnlicher Temperatur gerührt. Hierauf wird das überschüssige Oxalylchlorid ab destilliert und der Rückstand, nach Zugabe von 1000 Teilen Schwefelkohlenstoff, unter Rühren innert einer Stunde mit 250 Teilen- Aluminiumchlorid versetzt, wobei die Tem peratur bei 0 bis<B>10'</B> gehalten wird.
Man rührt nun noch längere Zeit bei gewöhnlicher Temperatur, erwärmt .dann langsam bis zum Sieden des Schwefelkohlenstoffes und belässt eine Stunde bei dieser Temperatur. Man trägt dann das Reaktionsprodukt in salzsäurehalti ges -Wasser aus. Nach dem Abtreiben des Schwefelkohlenstoffes wird filtriert und der Rückstand mit verdünnter Sololösung bei <B>50'</B> bis 60 .a-usgezogen; aus der Sodalösung wird das 1-Chlor-2 . 3-thionaphthisatin durch Salzsäure gefällt. -
Process for the production of a thionaphthisatin. It has been found that a new thionaphthisatin, 1-chloro-2,3-thionaphthisatin, is obtained if oxalyl chloride is allowed to act on 1-chloro-2-thiophthol, optionally with the addition of a condensing agent.
The 1-chloro-2 .3-thionaphthisatin forms a red powder, after being redissolved once from benzene, crystals with a melting point of 194 'are obtained.
Example: 194.5 parts of 1-chloro-2-thiona, -phtliol (colorless needles with a melting point of 51) are added to about 600 parts of oxalyl chloride while stirring at 0 to 10 and the mixture is stirred for 20 hours at normal 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 within one hour, the temperature being kept at 0 to 10 '.
The mixture is then stirred for a longer time at normal temperature, then heated slowly until the carbon disulfide boils and left at this temperature for an hour. The reaction product is then discharged into hydrochloric acid-containing water. After the carbon disulfide has been driven off, it is filtered and the residue is drawn off with dilute solo solution at <B> 50 '</B> to 60%; the 1-chloro-2 is made from the soda solution. 3-thionaphthisatin precipitated by hydrochloric acid. -
Claims (1)
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CH104924T | 1922-12-02 | ||
CH102033T | 1922-12-02 |
Publications (1)
Publication Number | Publication Date |
---|---|
CH104924A true CH104924A (en) | 1924-05-16 |
Family
ID=25706108
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CH104924D CH104924A (en) | 1922-12-02 | 1922-12-02 | Process for the production of a thionaphthisatin. |
Country Status (1)
Country | Link |
---|---|
CH (1) | CH104924A (en) |
-
1922
- 1922-12-02 CH CH104924D patent/CH104924A/en unknown
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