DE286855C - - Google Patents
Info
- Publication number
- DE286855C DE286855C DENDAT286855D DE286855DA DE286855C DE 286855 C DE286855 C DE 286855C DE NDAT286855 D DENDAT286855 D DE NDAT286855D DE 286855D A DE286855D A DE 286855DA DE 286855 C DE286855 C DE 286855C
- Authority
- DE
- Germany
- Prior art keywords
- hexaaminoarsenobenzene
- parts
- acid
- solution
- dinitrobenzene
- 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
- 239000002253 acid Substances 0.000 claims description 5
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 3
- JVBXVOWTABLYPX-UHFFFAOYSA-L sodium dithionite Chemical compound [Na+].[Na+].[O-]S(=O)S([O-])=O JVBXVOWTABLYPX-UHFFFAOYSA-L 0.000 claims description 3
- 239000011593 sulfur Substances 0.000 claims description 3
- 229910052717 sulfur Inorganic materials 0.000 claims description 3
- 150000007513 acids Chemical class 0.000 claims description 2
- VJWWIRSVNSXUAC-UHFFFAOYSA-N arsinic acid Chemical group O[AsH2]=O VJWWIRSVNSXUAC-UHFFFAOYSA-N 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- 125000000449 nitro group Chemical group [O-][N+](*)=O 0.000 claims description 2
- 238000012986 modification Methods 0.000 claims 1
- 230000004048 modification Effects 0.000 claims 1
- 239000000243 solution Substances 0.000 description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N hydrochloric acid Substances Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- QFUSCYRJMXLNRB-UHFFFAOYSA-N 2,6-dinitroaniline Chemical compound NC1=C([N+]([O-])=O)C=CC=C1[N+]([O-])=O QFUSCYRJMXLNRB-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000003929 acidic solution Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic Table
- C07F9/66—Arsenic compounds
- C07F9/70—Organo-arsenic compounds
- C07F9/74—Aromatic compounds
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Description
KAISERLICHESIMPERIAL
PATENTAMT.PATENT OFFICE.
PATENTSCHRIFTPATENT LETTERING
- JV* 286855 - KLASSE 12 #.'GRUPPE - JV * 286855 - CLASS 12 #. 'GROUP
Verfahren zur Darstellung eines Hexaaminoarsenobenzols.Process for the preparation of a hexaaminoarsenobenzene.
Zusatz zum Patent 286854.Addendum to patent 286854.
Patentiert im Deutschen Reiche vom 30. August 1913 ab. Längste Dauer: 4. März 1928.Patented in the German Empire on August 30, 1913. Longest duration: March 4, 1928.
Durch das Hauptpatent 286854 ist ein Verfahren zur Darstellung eines Hexaaminoarsenobenzols geschützt, welches darin besteht, daß man 4-Amino-3, 5-dinitrobenzol-i-arsinsäure stufenweise reduziert. Behandelt man 4-Amino-3, 5 - dinitrobenzol -1 - arsinsäure mit Metallen bzw. Metallsalzen, wie Zinn, Zink oder Zinnchlorür, in stark saurer Lösung, so führt die Reduktion unmittelbar zum Hexaaminoarsenobenzol. Versucht man jedoch die unmittelbare Reduktion mit einer zur Reduktion der Nitrogruppe und des Arsinsäurerestes ausreichenden Menge Natriumhydrosulfit auszuführen, so erhält man entgegen anderen aus der Literatur bekannten analogen Fällen (vgl. z. B. Patentschrift 224953, Kl. 12 q) zunächst ein schwefelhaltiges Zwischenprodukt. Dieses gibt auffallenderweise mit Alkali eine klare Lösung, so daß anscheinend die Reduktion nicht zu der gewünschten Hexaaminoverbindung geführt hat. Wie nun weiter gefunden wurde, liefert jedoch das erwähnte schwefelhaltige Zwischenprodukt beim Behandeln mit Säuren, zweckmäßig in der Wärme, unter Abspaltung von schwefliger Säure die Salze des Hexaaminoarsenobenzols. The main patent 286854 describes a process for the preparation of a hexaaminoarsenobenzene protected, which consists in that you 4-amino-3, 5-dinitrobenzene-i-arsic acid gradually reduced. Treating 4-amino-3, 5 - dinitrobenzene -1 - arsic acid with metals or metal salts, such as tin, zinc or tin chloride, in a strongly acidic solution, this leads to the Reduction directly to hexaaminoarsenobenzene. If you try the immediate one, however Reduction with an amount sufficient to reduce the nitro group and the arsinic acid residue To carry out the amount of sodium hydrosulfite is obtained, contrary to others, from the literature known analogous cases (see, for example, patent specification 224953, class 12 q) sulfur-containing intermediate. Strikingly, this gives a clear solution with alkali, so that apparently the reduction did not lead to the desired hexaamino compound Has. As has now been further found, however, the aforementioned sulfur-containing intermediate produces when treated with acids, expediently in the heat, with elimination of sulfurous acid, the salts of hexaaminoarsenobenzene.
Beispiel. ·■Example. · ■
3 Teile Dinitroaminobenzolarsinsäure werden in 60 Teilen Wasser unter Zusatz von 5,4 Teilen zweifach η-Natronlauge gelöst und unter kräftigem Rühren allmählich mit 35 Teilen Natriumhydrosulfit versetzt. Die Lösung wird entfärbt, und es beginnt bald die Abscheidung eines gelben flockigen Körpers, die nach kurzer Zeit beendet ist. Der Niederschlag wird abgesaugt, mit etwas Wasser gewaschen und in 50 Teilen Wasser suspendiert, das mit 20 Teilen vierfach η-Salzsäure angesäuert ist. Durch gelindes Erwärmen tritt allmählich unter Entweichen von schwefliger SäuVe Lösung ein. Man filtriert und fällt aus der salzsauren Lösung das Hexaaminoarsenobenzol mittels verdünnter Natronlauge aus. Die Base wird abfiltriert, mit Wasser gut ausgewaschen und nach den Angaben des Hauptpatents 286854 z. B. in die beständige Form ihres salzsauren Salzes übergeführt.3 parts of dinitroaminobenzolaric acid are dissolved in 60 parts of water with the addition of 5.4 parts twice dissolved η-sodium hydroxide solution and gradually adding 35 parts with vigorous stirring Sodium hydrosulfite added. The solution becomes discolored and precipitation soon begins of a yellow flaky body that ends after a short time. The precipitate is sucked off, washed with a little water and suspended in 50 parts of water, that with 20 parts fourfold η-hydrochloric acid is acidified. By gentle heating occurs gradually with escape of sulphurous acid solution. It is filtered and precipitated from the hydrochloric acid solution the hexaaminoarsenobenzene using dilute sodium hydroxide solution. The base is filtered off, Washed out well with water and according to the information of the main patent 286854 z. B. converted into the permanent form of their hydrochloric acid salt.
Claims (1)
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE286855T |
Publications (1)
Publication Number | Publication Date |
---|---|
DE286855C true DE286855C (en) | 1915-09-08 |
Family
ID=6059153
Family Applications (2)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
DENDAT286855D Expired DE286855C (en) | |||
DENDAT286854D Expired DE286854C (en) |
Family Applications After (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
DENDAT286854D Expired DE286854C (en) |
Country Status (1)
Country | Link |
---|---|
DE (2) | DE286854C (en) |
-
0
- DE DENDAT286855D patent/DE286855C/de not_active Expired
- DE DENDAT286854D patent/DE286854C/de not_active Expired
Also Published As
Publication number | Publication date |
---|---|
DE286854C (en) | 1900-01-01 |
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