US1023977A - Dye. - Google Patents

Dye. Download PDF

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Publication number
US1023977A
US1023977A US58085910A US1910580859A US1023977A US 1023977 A US1023977 A US 1023977A US 58085910 A US58085910 A US 58085910A US 1910580859 A US1910580859 A US 1910580859A US 1023977 A US1023977 A US 1023977A
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United States
Prior art keywords
acid
pyrazolone
methylene
dyeing
dye
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Legal status (The legal status 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 status listed.)
Expired - Lifetime
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US58085910A
Inventor
Max Weiler
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Bayer AG
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Individual
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Priority to US58085910A priority Critical patent/US1023977A/en
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D231/00Heterocyclic compounds containing 1,2-diazole or hydrogenated 1,2-diazole rings
    • C07D231/02Heterocyclic compounds containing 1,2-diazole or hydrogenated 1,2-diazole rings not condensed with other rings
    • C07D231/10Heterocyclic compounds containing 1,2-diazole or hydrogenated 1,2-diazole rings not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members
    • C07D231/14Heterocyclic compounds containing 1,2-diazole or hydrogenated 1,2-diazole rings not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
    • C07D231/18One oxygen or sulfur atom
    • C07D231/20One oxygen atom attached in position 3 or 5
    • C07D231/22One oxygen atom attached in position 3 or 5 with aryl radicals attached to ring nitrogen atoms
    • C07D231/261-Phenyl-3-methyl-5- pyrazolones, unsubstituted or substituted on the phenyl ring

Definitions

  • My invention relates to the manufacture and production of new dyestuffs of the aurin series, which are obtained by condensing in the presence of oxidizing agents methylene oxycarboxylic acids, especially 1nethylene-di-salicylic acid and methylenediortho-cresotinic acid with pyrazolones containing probably in their molecule the following group:
  • Methylene-di-ortho-cresotinic acid may be replaced by methylene-di-salicylic or methylene-di- 2. l-dioxybenzoic acid, etc., or by mixed methylene-di-hydroxy acids.
  • Methylene-di-ortho-cresotinic acid may be replaced by methylene-di-salicylic or methylene-di- 2. l-dioxybenzoic acid, etc., or by mixed methylene-di-hydroxy acids.
  • the hydrogenes of the two carboxylic-benzene nuclei may be further substituted by the methyland hydroxyl group.
  • the new dyes are dark powders soluble in dilute caustic soda lye generally with a red color, dyeing wool from acid baths generally from red to violet to brown shades, which can be chromed on the fiber.
  • the parts being by weight :21.1 parts of methylene-di-ortho-cresotinic acid and 12.8 parts of 3-methyl-l-phenyl-5-pyrazolone are mixed with 320 parts of strong sulfuric acid and the necessary quantity of nitrosyl sulfuric acid and then stirred at from 20- 45" C. until the quantity of the dyestuff produced is not further increased and the evolution of nitrogen oxids ceases.
  • the product of the reaction is poured on ice and the dyestuff is filtered off.
  • pyrazolones may be employed, 6. g. 3-methyl-5-pyrazolone, 3-methyl-1- para-sulfophenyl-5-pyrazolone, 3-methyl- 5- pyrazolone-l-beta napht-hyl 4.8 disulfonlc acid, 3 carboxy 1 phenyl-5-pyrazolone, 3- carboxy 5 pyrazolone 1 phenyl para-sulfonic acid, etc.
  • the dyeing can be done in the usual ways.
  • 001 is either dyed and treated with bichroinates after dyeing, or wool mordanted with chromium compounds is dyed, 0r uninordanted wool is dyed and niordanted in one operation from a bath containing both dyestutt and chrome niordant.
  • R means an aryl radical which dyestuffs are dark powders soluble in dilute caustic soda lye generally with a red color, dyeing wool from acid baths generally from red to violet to brown shades, which can be chromed after dyeing, substantially as described.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Coloring (AREA)

Description

Umrnn srarns PATENT OFFICE.
MAX WEILER, OF ELBERFELD, GERMANY, ASSIGNOR TO FARBENFABRIKEN VORlVL FRIEDR. BAYER & 00., OF ELBERFELD, GERMANY, A CORPORATION OF GERMANY.
DYE.
No Drawing.
Specification of Letters Patent.
Application filed September 7, 1910.
To aZZ whom it may concern Be it known that I, MAX WEILER, doctor of philosophy chemist, citizen of the German Empire, residing at Elberfeld, Germany, have invented new and useful Improvements in New Dye, of which the following is a specification.
My invention relates to the manufacture and production of new dyestuffs of the aurin series, which are obtained by condensing in the presence of oxidizing agents methylene oxycarboxylic acids, especially 1nethylene-di-salicylic acid and methylenediortho-cresotinic acid with pyrazolones containing probably in their molecule the following group:
0 R meaning the phenylor naphthyl radical,
fuming sulfuric acid may be used. Methylene-di-ortho-cresotinic acid may be replaced by methylene-di-salicylic or methylene-di- 2. l-dioxybenzoic acid, etc., or by mixed methylene-di-hydroxy acids. Instead of 3-methyl- 1-phenyl-5-pyrazolone mentioned in the exand R the methylor carboxyl group; the hydrogenes of the two carboxylic-benzene nuclei may be further substituted by the methyland hydroxyl group.
The new dyes are dark powders soluble in dilute caustic soda lye generally with a red color, dyeing wool from acid baths generally from red to violet to brown shades, which can be chromed on the fiber.
In order to illustrate the new process more fully the following example is given, the parts being by weight :21.1 parts of methylene-di-ortho-cresotinic acid and 12.8 parts of 3-methyl-l-phenyl-5-pyrazolone are mixed with 320 parts of strong sulfuric acid and the necessary quantity of nitrosyl sulfuric acid and then stirred at from 20- 45" C. until the quantity of the dyestuff produced is not further increased and the evolution of nitrogen oxids ceases. The product of the reaction is poured on ice and the dyestuff is filtered off. It is a yellowish-brown powder soluble in hot water with an orange color, in dilute caustic soda lye with an orange-red color, capable of dyeing wool in orange shades which on chroming turn into an intense brownish-orange and is probably obtained according to the following formula:
ample other pyrazolones may be employed, 6. g. 3-methyl-5-pyrazolone, 3-methyl-1- para-sulfophenyl-5-pyrazolone, 3-methyl- 5- pyrazolone-l-beta napht-hyl 4.8 disulfonlc acid, 3 carboxy 1 phenyl-5-pyrazolone, 3- carboxy 5 pyrazolone 1 phenyl para-sulfonic acid, etc.
The dyeing can be done in the usual ways.
001 is either dyed and treated with bichroinates after dyeing, or wool mordanted with chromium compounds is dyed, 0r uninordanted wool is dyed and niordanted in one operation from a bath containing both dyestutt and chrome niordant.
I claim 1. The herein described new dyestuffs, being condensation products of methylene-dioxycarboxylic acids and pyrazolones containing probably in their molecule the following characteristic group:
OH O R COOH (X91 pyrazolone in which R means an aryl radical which dyestuffs are dark powders soluble in dilute caustic soda lye generally with a red color, dyeing wool from acid baths generally from red to violet to brown shades, which can be chromed after dyeing, substantially as described.
2. The herein described new dyestuff having probably the following formula:
on 0H3 my hand in the presence of two subscribing witnesses.
MAX WEILER. [n s] Witnesses CHAS. J. WRIGHT,
lVALTER VONNEGUT.
Copies of this patent may be obtained for five cents each, by addressing the Commissioner of latents, Washington, D. C.
US58085910A 1910-09-07 1910-09-07 Dye. Expired - Lifetime US1023977A (en)

Priority Applications (1)

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US58085910A US1023977A (en) 1910-09-07 1910-09-07 Dye.

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