CH177264A - Process for the preparation of a new intermediate dye. - Google Patents

Process for the preparation of a new intermediate dye.

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Publication number
CH177264A
CH177264A CH177264DA CH177264A CH 177264 A CH177264 A CH 177264A CH 177264D A CH177264D A CH 177264DA CH 177264 A CH177264 A CH 177264A
Authority
CH
Switzerland
Prior art keywords
parts
preparation
new intermediate
hydroquinone
intermediate dye
Prior art date
Application number
Other languages
German (de)
Inventor
Limited Imperial Ch Industries
Original Assignee
Ici Ltd
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 Ici Ltd filed Critical Ici Ltd
Publication of CH177264A publication Critical patent/CH177264A/en

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Description

  

  Verfahren zur Herstellung eines neuen     Farbstoffzwischenproduktes.       Es wurde gefunden, dass man ein neues  und nützliches     Zwischenprodukt    erhält, wenn       inan        Hydrochinon    mit.     Äthylenchlorhydrin     kondensiert, den resultierenden     Hydrochinon-          di-(ss-liydroxyätliyl)-äther        mononitriert.    und  die so erhaltene     Nitroverbindung    zum Amin  reduziert. Das Endprodukt hat einen  Schmelzpunkt von<B>1322</B> bis 134   C.  



  <I>Beispiel:</I>  275 Teile     Hydrochinon    und 205 Teile       Natriumhy        droxyd    werden in 1000 Teilen  Wasser aufgelöst und auf 45   C erhitzt.  25 Teile gefällte Kreide werden zugesetzt,  worauf eine Auflösung von 403 Teilen       Äthylenehlorhydrin    in 806 Teilen Wasser  folgt. Das Gemisch wird zum Kochen ge  bracht und 5 Stunden unter     Rückfluss    und       hinrühren    gekocht. Das Gemisch wird zur  Entfernung der Kreide     abgefiltert,    180 Teile       Natriumchlorid    werden dem heissen Filtrat  zugesetzt und dieses wird unter Umrühren    auf 25   C     kühlen    gelassen.

   Der so erhaltene       Hydrochinon-di-(ss-hydroxyäthyl)-äther    wird       abfiltriert    und gut trocken gelegt.  



       1.16    Teile     86,3/"0    Salpetersäure und 214  Teile Wasser werden gemischt und 198 Teile       Hydrochinon-di-(ss-hydroxyäthyl)-äther    wer  den in einer halben Stunde bei 30 bis 35   C  als eine wässerige, 44 Teile Wasser enthal  tende Paste zugesetzt. Das Gemisch wird  drei Stunden bei 30 bis 35   C umgerührt  und wird dann mit 500 Teilen Wasser ver  dünnt und auf     Brilliant    Gelbpapier durch  zirka 130 Teile 32 % wässerigen Natrium  hydroxyd alkalisch gemacht.

   Weitere 120  Teile 32 % wässerigem     Natriumhydroxyd     werden zugesetzt und hierauf 40 Teile  Schwefel und 300 Teile     Natriumsulfidkry-          stalle.    Das Gemisch wird dann unter leich  tem Kochen 5 Stunden lang umgerührt und  unter Rühren auf 25   C kühlen gelassen.  Der ausgefallene     Aminohydrochinon-di-(ss-          hydroxyäthyl)-äther    wird     abfiltriert,    mit 200      Teilen kaltem Wasser gewaschen und ge  trocknet.



  Process for the preparation of a new intermediate dye. It has been found that a new and useful intermediate is obtained when using hydroquinone. Ethylene chlorohydrin condenses, the resulting hydroquinone di- (ss-liydroxyätliyl) ether is mononitrated. and reducing the nitro compound thus obtained to the amine. The end product has a melting point of <B> 1322 </B> to 134 C.



  <I> Example: </I> 275 parts of hydroquinone and 205 parts of sodium hydroxide are dissolved in 1000 parts of water and heated to 45.degree. 25 parts of precipitated chalk are added, followed by a dissolution of 403 parts of ethylene chlorohydrin in 806 parts of water. The mixture is brought to the boil and refluxed and stirred for 5 hours. The mixture is filtered off to remove the chalk, 180 parts of sodium chloride are added to the hot filtrate and this is allowed to cool to 25 ° C. while stirring.

   The hydroquinone di- (β-hydroxyethyl) ether thus obtained is filtered off and dried thoroughly.



       1.16 parts of 86.3 / "0 nitric acid and 214 parts of water are mixed and 198 parts of hydroquinone di (ss-hydroxyethyl) ether are used in half an hour at 30 to 35 C as an aqueous paste containing 44 parts of water The mixture is stirred for three hours at 30 to 35 ° C. and is then diluted with 500 parts of water and made alkaline on Brilliant Yellow paper by about 130 parts of 32% aqueous sodium hydroxide.

   A further 120 parts of 32% aqueous sodium hydroxide are added, followed by 40 parts of sulfur and 300 parts of sodium sulfide crystals. The mixture is then stirred with gentle boiling for 5 hours and allowed to cool to 25 ° C. with stirring. The precipitated aminohydroquinone di (ss-hydroxyethyl) ether is filtered off, washed with 200 parts of cold water and dried.

Claims (1)

PATENTANSPRUCH: Verfahren zur Herstellung eines neuen Farbstoffzwischenproduktes, dadurch ge kennzeichnet, dass man Hydrochinon mit Athylenehlorhydrin kondensiert, den resul tierenden Hydrochinon-di-(,ss-hydroxyäthyl)- äther mononitriert und die Nitroverbindung zum Aminohydrochixion-di-(ss-hydroxyäthyl)- äther, welcher den Schmelzpunkt 132 bis 134' C zeigt, reduziert. PATENT CLAIM: Process for the production of a new intermediate dye product, characterized in that hydroquinone is condensed with Ethylenehlorhydrin, the resulting hydroquinone di - (, ss-hydroxyethyl) - ether is mononitrated and the nitro compound to aminohydrochixion-di- (ss-hydroxyethyl) - ether, which has a melting point of 132 to 134 ° C, is reduced.
CH177264D 1933-07-06 1934-07-03 Process for the preparation of a new intermediate dye. CH177264A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
GB177264X 1933-07-06

Publications (1)

Publication Number Publication Date
CH177264A true CH177264A (en) 1935-05-31

Family

ID=10100149

Family Applications (1)

Application Number Title Priority Date Filing Date
CH177264D CH177264A (en) 1933-07-06 1934-07-03 Process for the preparation of a new intermediate dye.

Country Status (1)

Country Link
CH (1) CH177264A (en)

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