DE661750C - Process for the preparation of gold compounds from keratin breakdown products - Google Patents
Process for the preparation of gold compounds from keratin breakdown productsInfo
- Publication number
- DE661750C DE661750C DESCH107649D DESC107649D DE661750C DE 661750 C DE661750 C DE 661750C DE SCH107649 D DESCH107649 D DE SCH107649D DE SC107649 D DESC107649 D DE SC107649D DE 661750 C DE661750 C DE 661750C
- Authority
- DE
- Germany
- Prior art keywords
- gold
- keratin
- preparation
- solution
- water
- Prior art date
- 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
Links
- 102000011782 Keratins Human genes 0.000 title claims description 12
- 108010076876 Keratins Proteins 0.000 title claims description 12
- 150000002344 gold compounds Chemical class 0.000 title claims description 9
- 238000000034 method Methods 0.000 title claims description 5
- 238000002360 preparation method Methods 0.000 title claims description 3
- 230000015556 catabolic process Effects 0.000 title description 4
- 239000000243 solution Substances 0.000 claims description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 8
- 229940044660 gold keratinate Drugs 0.000 claims description 7
- 108010079530 gold keratinate Proteins 0.000 claims description 7
- 230000002378 acidificating effect Effects 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 238000005903 acid hydrolysis reaction Methods 0.000 claims description 4
- 229910021529 ammonia Inorganic materials 0.000 claims description 4
- 150000002343 gold Chemical class 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- 239000007857 degradation product Substances 0.000 claims description 3
- 239000003960 organic solvent Substances 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 2
- 238000006386 neutralization reaction Methods 0.000 claims description 2
- 239000003929 acidic solution Substances 0.000 claims 1
- 239000003513 alkali Substances 0.000 claims 1
- GEHJBWKLJVFKPS-UHFFFAOYSA-N bromochloroacetic acid Chemical compound OC(=O)C(Cl)Br GEHJBWKLJVFKPS-UHFFFAOYSA-N 0.000 claims 1
- 238000001226 reprecipitation Methods 0.000 claims 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 18
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 8
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 8
- 239000010931 gold Substances 0.000 description 8
- 229910052737 gold Inorganic materials 0.000 description 8
- 239000000047 product Substances 0.000 description 8
- FDWREHZXQUYJFJ-UHFFFAOYSA-M gold monochloride Chemical compound [Cl-].[Au+] FDWREHZXQUYJFJ-UHFFFAOYSA-M 0.000 description 5
- 239000002244 precipitate Substances 0.000 description 4
- 239000007788 liquid Substances 0.000 description 3
- 210000002268 wool Anatomy 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- AZMMUMQYPBKXHS-UHFFFAOYSA-N gold sodium Chemical compound [Na].[Au] AZMMUMQYPBKXHS-UHFFFAOYSA-N 0.000 description 2
- 210000004209 hair Anatomy 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- 159000000000 sodium salts Chemical class 0.000 description 2
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 150000001447 alkali salts Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 210000003284 horn Anatomy 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000001632 sodium acetate Substances 0.000 description 1
- 235000017281 sodium acetate Nutrition 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 230000001225 therapeutic effect Effects 0.000 description 1
- 125000003396 thiol group Chemical group [H]S* 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K38/00—Medicinal preparations containing peptides
- A61K38/01—Hydrolysed proteins; Derivatives thereof
- A61K38/012—Hydrolysed proteins; Derivatives thereof from animals
- A61K38/014—Hydrolysed proteins; Derivatives thereof from animals from connective tissue peptides, e.g. gelatin, collagen
- A61K38/015—Hydrolysed proteins; Derivatives thereof from animals from connective tissue peptides, e.g. gelatin, collagen from keratin
Landscapes
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Medicinal Chemistry (AREA)
- Proteomics, Peptides & Aminoacids (AREA)
- Chemical & Material Sciences (AREA)
- Bioinformatics & Cheminformatics (AREA)
- Immunology (AREA)
- Biomedical Technology (AREA)
- Pharmacology & Pharmacy (AREA)
- Zoology (AREA)
- Epidemiology (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Cosmetics (AREA)
Description
Verfahren zur Darstellung von Goldverbindungen von Keratinabbauprodukten Es ist bereits bekannt, daß man aus Keratinsubstanzen durch saure Hydrolyse bei gleichzeitiger oder anschließender Reduktion albumoseartige, Sulfhydrylgruppen enthaltende Keratinabbauprodukte gewinnen kann, die bei der Umsetzung mit Goldsalzen in üblicher Weise wasserlösliche, therapeutisch verwendbare Goldverbindungen ergeben. Die hierbei angewendete Reduktion gestaltet das Verfahren umständlich; dazu kommt noch, daß die Ausbeuten an wirksamen Erzeugnissen sehr niedrige sind, da bei der Reduktion ein weitgehender Abbau der Keratinsubstanzen stattfindet.Process for the preparation of gold compounds from keratin breakdown products It is already known that keratin substances can be obtained by acid hydrolysis simultaneous or subsequent reduction containing albumose-like sulfhydryl groups Keratin breakdown products can be obtained when implemented with gold salts in the usual way Wise water-soluble, therapeutically useful gold compounds result. The one here the applied reduction makes the process cumbersome; there is also that the yields of active products are very low because of the reduction extensive degradation of the keratin substances takes place.
Es wurde nun gefunden, daß man zu therapeutisch sehr wertvollen, wasserlöslichen, ungiftigen, komplexen Goldverbindungen in guter Ausbeute gelangen kann, wenn man die nach der Säurehydrolyse .erhaltenen Keratinabbauprodukte unmittelbar mit Goldsalzen in bisher unbekannte Goldverbindungen überführt. Dabei hat es sich als vorteilhaft herausgestellt, daß man nach der Säurehydrolyse, z. B. mit Salzsäure, das saure Hydrolysat mit alkalischen Stoffen, zweckmäßig mit Ammoniak, neutralisiert.It has now been found that therapeutically very valuable, water-soluble, non-toxic, complex gold compounds can be obtained in good yield if one the keratin degradation products obtained after acid hydrolysis directly with gold salts converted into previously unknown gold compounds. It has been found to be beneficial found that after acid hydrolysis, for. B. with hydrochloric acid, the acidic Hydrolyzate neutralized with alkaline substances, expediently with ammonia.
Die neuen Goldverbindungen werden nach Umwandlung in ihre Alkalisalze aus der Umsetzungslösung durch Zusatz von mit Wasser mischbaren organischen Lösungsmitteln, z. B. durch Zusatz von Alkohol, ausgefällt und stellen schwach gelb gefärbte Produkte dar. Sie lösen sich leicht in Wasser und sind trotz ihrer einfachen Herstellungsweise den bekannten Goldkeratinverbindungen in therapeutischer Hinsicht gleichwertig oder sogar noch überlegen. Beispiel i ioo g Keratin (Haare, Wolle, Horn usw.) werden mit 400 g 18 O/oiger Salzsäure im Wasserbad erhitzt, bis das gesamte Keratin in Lösung gegangen ist. Darauf wird das Hydrolysat durch Zusatz von konzentriertem Ammoniak neutralisiert und von ungelösten Bestandteilen abfiltriert.The new gold compounds are converted into their alkali salts from the reaction solution by adding water-miscible organic solvents, z. B. by adding alcohol, precipitated and make pale yellow colored products They dissolve easily in water and, despite their simple manufacturing process, are or equivalent to the known gold keratin compounds in therapeutic terms even superior. Example ioo g of keratin (hair, wool, horn, etc.) will be heated with 400 g of 18% hydrochloric acid in a water bath until all of the keratin is in Solution has gone. The hydrolyzate is then concentrated by adding concentrated Ammonia is neutralized and undissolved components are filtered off.
In das neutrale, abgekühlte Hydrolysat wird eine Lösung von Goldchlorid in Wasser eingetragen, bis der zunächst ausfallende Niederschlag gerade noch in Lösung geht. Hierzu sind etwa 4,5 bis 5,0 g Goldchlorid erforderlich. Die nunmehr sauer gewordene Lösung wird mit Natronlauge neutralisiert und in die fünffache Menge Alkohol gegossen, wobei sich das entstandene Goldkeratinat in sich zusammenballenden Flokken abscheidet. Man läßt absitzen und gießt die alkoholische Flüssigkeit ab. Der Niederschlag wird zur Reinigung unter Zusatz von wenig Natronlauge in Wasser gelöst und erneut durch Eingießen in Alkohol, gegebenenfalls unter Zusatz von etwas Natriumacetatlösung, gefällt. Nach zweimaligem Umfällen wird die Goldverbindung als feinpulveriges, nur schwach gelb gefärbtes Produkt erhalten, das etwa 6°/o Gold enthält.A solution of gold chloride in water is added to the neutral, cooled hydrolyzate until the precipitate that initially separates out just about dissolves. About 4.5 to 5.0 g of gold chloride are required for this. The solution, which has now become acidic, is neutralized with sodium hydroxide solution and poured into five times the amount of alcohol, with the resulting gold keratinate being deposited in clusters of flakes. It is allowed to settle and the alcoholic liquid is poured off. For purification, the precipitate is dissolved in water with the addition of a little sodium hydroxide solution and precipitated again by pouring it into alcohol, optionally with the addition of a little sodium acetate solution. After reprecipitating twice, the gold compound is obtained as a finely powdered product, only slightly yellow in color, which contains about 6% gold.
Die Ausbeute beträgt 2o bis 25 g aus ioo g Keratin.The yield is from 20 to 25 g from 100 g of keratin.
Beispiel 2 ioo g Haare werden in der gleichen Weise wie in Beispiel i mit Salzsäure abgebaut und die Hydrolysenflüssigkeit mit Ammoniak neutralisiert. In die neutrale Lösung werden sodann 7,5 g Goldchlorid, in 50 ccm Wasser gelöst, eingetragen, wobei das entstandene Goldkeratinat ausfällt: Durch Neutralisation mit Natronlauge, wird das Goldkeratinat als Natriumsalz in Lti-', sung gebracht und durch Eingießen der LösuüK in die fünffache Menge Alkohol die Goldverbindung gefällt. Zur Reinigung wird diese Verbindung mehrmals in Wasser gelöst und wieder mit Alkohol gefällt. Die Ausbeute an Goldkeratinat beträgt 2o g: Das Erzeugnis enthält 13 bis 1q°/0 Gold.Example 2 100 g of hair are broken down in the same way as in Example 1 with hydrochloric acid and the hydrolysis liquid is neutralized with ammonia. 7.5 g of gold chloride, dissolved in 50 cc of water, are then added to the neutral solution, the gold keratinate formed precipitating: the gold keratinate is brought into solution as the sodium salt by neutralization with sodium hydroxide solution and the solution is poured into the five times the amount of alcohol that pleases the gold compound. For cleaning, this compound is dissolved several times in water and precipitated again with alcohol. The yield of gold keratinate is 20 g: The product contains 13 to 1q% gold.
Durch Zusatz von noch größeren Mengen Goldchlorid zur Hydrolysenflüssigkeit können Goldkerätinate mit einem Goldgehalt bis zu 331)/, erhalten werden.By adding even larger amounts of gold chloride to the hydrolysis liquid gold keratinates with a gold content of up to 331) /, can be obtained.
Beispiel 3 iöo g Wolle werden mit 440 g einer 2o °/°igen Salzsäure im Wasserbad so lange erhitzt, bis die Wolle in der Hauptsache in Lösung gegangen ist. Hierauf wird abgekühlt, das saure Hydrolysat mit so viel einer 33 °/°lgen Natronlauge abgestumpft, daß die Reaktion nur noch lackmussauer, aber nicht mehr kongosauer ist, und von ungelösten Bestandteilen abfiltriert. In das Hydrolysät werden alsdann 45 ccm einer 2o°/°igen wässerigen Lösung von Goldchlorid (Goldgehalt=5o°/°) unter Rühren allmählich eingetragen und die hierbei ausfallende Goldkeratinsäure durch Zugabe von Natronlauge bis zur schwach alkalischen Reaktion als Natriumsalz in Lösung gebracht. Die Lösung wird alsdann filtriert und das Filtrat in die siebenfache Menge Alkohol eingerührt, wobei das Nätrium-Goldkeratinat zunächst als leimähnliches Produkt ausfällt. Zur Reinigung wird dieses Produkt noch zwei- bis dreimal unter Zusatz von wenig Natronlauge in Wasser gelöst und wieder mit Alkohol gefällt. Die zuletzt erhaltene körnige etsfällung wird von dem Alkohol abgesaugt, mit ='lkohol und Äther gewaschen und im Vakuum bei 7o' getrocknet. Es werden 23 g eines hellgelben Natrium-Goldkeratinats mit einem Goldgehalt von etwa 14.% erhalten.Example 3 100 g of wool are mixed with 440 g of 20% hydrochloric acid heated in a water bath until the wool has mainly dissolved is. It is then cooled, the acidic hydrolyzate with as much a 33% sodium hydroxide solution dulled, that the reaction was now only a lackmust wall, but no longer an acidic Congo is, and filtered off from undissolved constituents. Then into the hydrolyzate 45 ccm of a 20 ° / ° aqueous solution of gold chloride (gold content = 50 ° / °) below Stirring gradually entered and the gold keratinic acid which precipitates through Addition of sodium hydroxide solution until a weakly alkaline reaction is achieved as the sodium salt in solution brought. The solution is then filtered and the filtrate in seven times the amount Alcohol is stirred in, the sodium gold keratinate initially as a glue-like product fails. For cleaning, this product is added two or three times dissolved in water by a little sodium hydroxide solution and precipitated again with alcohol. The last The granular precipitate obtained is sucked off from the alcohol, with alcohol and ether washed and dried in vacuo at 70 '. There are 23 g of a light yellow sodium gold keratinate with a gold content of about 14%.
Claims (2)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DESCH107649D DE661750C (en) | 1935-08-03 | 1935-08-03 | Process for the preparation of gold compounds from keratin breakdown products |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DESCH107649D DE661750C (en) | 1935-08-03 | 1935-08-03 | Process for the preparation of gold compounds from keratin breakdown products |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| DE661750C true DE661750C (en) | 1938-06-25 |
Family
ID=7448439
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DESCH107649D Expired DE661750C (en) | 1935-08-03 | 1935-08-03 | Process for the preparation of gold compounds from keratin breakdown products |
Country Status (1)
| Country | Link |
|---|---|
| DE (1) | DE661750C (en) |
-
1935
- 1935-08-03 DE DESCH107649D patent/DE661750C/en not_active Expired
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