DE210693C - - Google Patents
Info
- Publication number
- DE210693C DE210693C DENDAT210693D DE210693DA DE210693C DE 210693 C DE210693 C DE 210693C DE NDAT210693 D DENDAT210693 D DE NDAT210693D DE 210693D A DE210693D A DE 210693DA DE 210693 C DE210693 C DE 210693C
- Authority
- DE
- Germany
- Prior art keywords
- derivatives
- glyoxylic acid
- acid
- phenylglycine
- lead
- 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.)
- Active
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- HHLFWLYXYJOTON-UHFFFAOYSA-N Glyoxylic acid Natural products OC(=O)C=O HHLFWLYXYJOTON-UHFFFAOYSA-N 0.000 claims description 14
- MUBZPKHOEPUJKR-UHFFFAOYSA-N oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 9
- ZGUNAGUHMKGQNY-UHFFFAOYSA-N α-phenylglycine Chemical compound OC(=O)C(N)C1=CC=CC=C1 ZGUNAGUHMKGQNY-UHFFFAOYSA-N 0.000 claims description 5
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 claims description 4
- 229910052753 mercury Inorganic materials 0.000 claims description 4
- 235000006408 oxalic acid Nutrition 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 2
- 238000005868 electrolysis reaction Methods 0.000 claims 1
- 150000002148 esters Chemical class 0.000 claims 1
- AMANDCZTVNQSNB-UHFFFAOYSA-N glyoxamide Chemical compound NC(=O)C=O AMANDCZTVNQSNB-UHFFFAOYSA-N 0.000 claims 1
- 230000004048 modification Effects 0.000 claims 1
- 238000006011 modification reaction Methods 0.000 claims 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 8
- 239000003792 electrolyte Substances 0.000 description 4
- PQJZHMCWDKOPQG-UHFFFAOYSA-N 2-anilino-2-oxoacetic acid Chemical compound OC(=O)C(=O)NC1=CC=CC=C1 PQJZHMCWDKOPQG-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000000875 corresponding Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- LMMSPVMUSOMTDD-UHFFFAOYSA-N ethyl oxane-2-carboxylate Chemical compound CCOC(=O)C1CCCCO1 LMMSPVMUSOMTDD-UHFFFAOYSA-N 0.000 description 1
- 230000002349 favourable Effects 0.000 description 1
- 239000002198 insoluble material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B3/00—Electrolytic production of organic compounds
- C25B3/20—Processes
- C25B3/25—Reduction
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
Description
KAISERLICHESIMPERIAL
PATENTAMT.PATENT OFFICE.
PATENTSCHRIFTPATENT LETTERING
-M 210693-KLASSE 12o. GRUPPE -M 210693-CLASS 12o. GROUP
KINZLBERGER & CO. in PRAG.KINZLBERGER & CO. in Prague.
elektrolytische Reduktion.electrolytic reduction.
Zusatz.zum Patente 163842 vom 10. September 1903.Addition to patent 163842 of September 10, 1903.
Patentiert im Deutschen Reiche vom 14. August 1904 ab. Längste Dauer: 9. September 1918.Patented in the German Empire on August 14, 1904. Longest duration: September 9, 1918.
Das Hauptpatent betrifft ein Verfahren zur Reduktion von Oxalsäure und ihren Derivaten zu Glyoxylsäure, und ihren entsprechenden Derivaten, sowie von Oxanilsäure und ihren Derivaten zu Phenylglycin bzw. dessen Derivaten durch elektrolytische Zersetzung an der Kathode unter Verwendung von Bleielektroden und von Schwefelsäure als Elektrolyt.The main patent relates to a process for reducing oxalic acid and its derivatives to glyoxylic acid, and its corresponding derivatives, and of oxanilic acid and its Derivatives to phenylglycine or its derivatives by electrolytic decomposition at the Cathode using lead electrodes and sulfuric acid as electrolyte.
Versuche haben nun gelehrt, daß der Verlauf der Reaktion nicht an die Verwendung von Bleielektroden gebunden ist, sondern daß Glyoxylsäure bzw. Phenylglycin und ihre Derivate auch bei Benutzung sonstiger, von dem schwefelsaxiren Elektrolyten nicht angreifbarer Elektroden in guter Ausbeute entstehen. Insbesondere wurden günstige Ergebnisse erzielt, wenn neben einer Anode aus Blei oder einem anderen unlöslichen Material eine Quecksilberkathode benutzt wurde. Begreiflicherweise müssen für jedes besondere Elektrodenmaterial die geeigneten Versuchsbedingungen ·—· Stromstärke und -spannung, Dauer des Stromdurchganges usf. — festgestellt werden.Experiments have now taught that the course of the reaction does not adhere to the use is bound by lead electrodes, but that glyoxylic acid or phenylglycine and their Derivatives also when using other electrolytes that are not vulnerable to sulfur-saxic electrolytes Electrodes are produced in good yield. In particular, favorable results have been achieved if in addition to an anode made of lead or some other insoluble material, a mercury cathode was used. It is understandable that the appropriate test conditions must be used for each particular electrode material. Current strength and voltage, duration of current passage, etc. - can be determined.
Darstellung von Phenylglycin. 5 Gewichtsteile Oxanilsäureäthylester werden in 100 Gewichtsteilen 80 prozentiger Schwefelsäure gelöst und mit einem Strom von 3 Amp. bei einer Stromdichte von 3 Amp. auf den Quadratdezimeter elektrolysiert. Man erhält an der Quecksilberkathode Phenylglycin in vorzüglicher Ausbeute.Presentation of phenylglycine. 5 parts by weight of ethyl oxanate are used in 100 parts by weight 80 percent sulfuric acid dissolved and with a current of 3 Amp. At a current density of 3 Amp. To the square decimeter electrolyzed. Phenylglycine is obtained in excellent form on the mercury cathode Yield.
Darstellung von Glyoxylsäure. Die Kathode besteht aus Quecksilber, die Anode aus Blei. Erstere ist von einer Lösung von Oxalsäure in 21Z2PrOZeUtIgCr Schwefelsäure, letztere von 5 prozentiger Schwefelsäure _ umgeben. Bei 61Z2 Amp. Stromstärke, 3 Amp. Stromdichte, 7,5 Volt Spannung und einer Temperatur von 5° erhält man Ausbeuten an Glyoxylsäure, welche 80 bis 85 Prozent der theoretischen betragen. Representation of glyoxylic acid. The cathode is made of mercury and the anode is made of lead. The former is surrounded by a solution of oxalic acid in 2 1 Z 2 PrOZeUtIgCr sulfuric acid, the latter by 5 percent sulfuric acid. At 6 1 Z 2 amp. Current intensity, 3 amp. Current density, 7.5 volt voltage and a temperature of 5 °, yields of glyoxylic acid are obtained which are 80 to 85 percent of the theoretical.
3535
4040
4545
Darstellung von Glyoxylsäure. Die Elektrolyte sind die unter Beispiel 2 angeführten. Als Elektroden dienen eine Kohlenkathode und eine Bleianode. Die Stromstärke beträgt 2 Amp., die Stromdichte 2 Amp., die Spannung 3,7 Volt und die Temperatur 50. Unter diesen Arbeitsbedingungen erhält man Glyoxylsäure in einer Ausbeute von 80 Prozent der theoretischen.Representation of glyoxylic acid. The electrolytes are those listed in Example 2. A carbon cathode and a lead anode serve as electrodes. The current intensity is 2 amps, the current density 2 amps, the voltage 3.7 volts and the temperature 50 . Under these working conditions, glyoxylic acid is obtained in a yield of 80 percent of the theoretical.
Claims (1)
Publications (1)
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Family
ID=472556
Family Applications (1)
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