DE555002C - Process for the preparation of a compound from theobromine calcium and calcium nitrite - Google Patents

Process for the preparation of a compound from theobromine calcium and calcium nitrite

Info

Publication number
DE555002C
DE555002C DEK120377D DEK0120377D DE555002C DE 555002 C DE555002 C DE 555002C DE K120377 D DEK120377 D DE K120377D DE K0120377 D DEK0120377 D DE K0120377D DE 555002 C DE555002 C DE 555002C
Authority
DE
Germany
Prior art keywords
calcium
theobromine
compound
nitrite
preparation
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
Application number
DEK120377D
Other languages
German (de)
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
HANS P KAUFMANN DR
Original Assignee
HANS P KAUFMANN DR
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 HANS P KAUFMANN DR filed Critical HANS P KAUFMANN DR
Priority to DEK120377D priority Critical patent/DE555002C/en
Application granted granted Critical
Publication of DE555002C publication Critical patent/DE555002C/en
Expired legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D473/00—Heterocyclic compounds containing purine ring systems
    • C07D473/02—Heterocyclic compounds containing purine ring systems with oxygen, sulphur, or nitrogen atoms directly attached in positions 2 and 6
    • C07D473/04—Heterocyclic compounds containing purine ring systems with oxygen, sulphur, or nitrogen atoms directly attached in positions 2 and 6 two oxygen atoms
    • C07D473/06—Heterocyclic compounds containing purine ring systems with oxygen, sulphur, or nitrogen atoms directly attached in positions 2 and 6 two oxygen atoms with radicals containing only hydrogen and carbon atoms, attached in position 1 or 3
    • C07D473/10—Heterocyclic compounds containing purine ring systems with oxygen, sulphur, or nitrogen atoms directly attached in positions 2 and 6 two oxygen atoms with radicals containing only hydrogen and carbon atoms, attached in position 1 or 3 with methyl radicals in positions 3 and 7, e.g. theobromine

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical And Physical Treatments For Wood And The Like (AREA)
  • Preventing Corrosion Or Incrustation Of Metals (AREA)

Description

Verfahren zur Herstellung einer Verbindung aus Theobromin-Calcium und Calciumnitrit Durch das Patent 548 373 wird ein Verfahren zur Herstellung einer Verbindung aus Calciumnitrit und Theobromin-Calciuni geschützt, das darin besteht, daß man (las Calciumsalz des Theobromins (oder Theobromin und Calciumhydroxyd) mit Calciumnitrit bei Gegenwart von Wasser zusammenbringt und die erhaltene Lösung unter Verwendung eines Vakuums zur Trockne eindampft. Es wurde nun gefunden, daß man zu dem gleichen Komplexsalz kommen kann, wenn man frisch dargestelltes und in Wasser unlösliches Tlieobromin-Calcium in konzentrierte Lösungen von Calciumnitrit bei Zimmertemperatur unter gutem Rühren einträgt. Das Reaktionsprodukt wird nach scharfem Absaugen auf der N utsche auf dem Tonteller getrocknet. Nachdem es pulverförmig geworden ist, extrahiert man es im Soxhletapparat mit Alkohol, wodurch das überschüssige Calciumnitrit herausgelöst wird. Es hinterbleibt ein auch bei verschiedenen Überschüssen von Calciumnitrit stets gleichmäßig zusammengesetztes Komplexsalz. Neben eingelagertem Wasser enthält es Theobromin-Calcium und Calciunmitrit im molekularen Verhältnis. In Wasser ist es leicht löslich, doch zersetzen sich die verdünnten Lösungen beim Stehen nach und nach, indem der Komplex wieder zerfällt. Auf dem beschriebenen Wege wird die neue Verbindung in einer Form erhalten, die sich leicht abfiltrieren und trocknen läßt, während bei dem Verfahren des Hauptpatents 548 373 die nach dem Zusammengeben der Komponenten entstehende Lösung zunächst eingedampft und dann unter Verwendung eines Vakuums in dünner Schicht getrocknet werden muß. Das obenerwähnte Waschendes Niederschlags mit Alkohol ist für den Fall vorgesehen, daß eine völlig reine Verbindung notwendig sein sollte. Es erübrigt sich dabei eine Gehaltsbestimmung der Ausgangsstoffe, die in Anbetracht des schwankenden Wassergehaltes der letzteren bei dem Verfahren des Hauptpatents unerläßlich ist.Process for the preparation of a compound from theobromine calcium and calcium nitrite By the patent 548,373 a process for the preparation of a Protected compound of calcium nitrite and theobromine calciuni, which consists in that one (read calcium salt of theobromine (or theobromine and calcium hydroxide) with Calcium nitrite brings together in the presence of water and the resulting solution under Using a vacuum to evaporate to dryness. It has now been found that one too The same complex salt can come from freshly rendered and immersed in water insoluble tlieobromine calcium in concentrated solutions of calcium nitrite Enters room temperature with thorough stirring. The reaction product is after sharp Vacuuming on the groove dried on the clay plate. After it's powdered it is extracted in the Soxhlet apparatus with alcohol, which removes the excess Calcium nitrite is dissolved out. It lingers even with various surpluses of calcium nitrite always an evenly composed complex salt. In addition to stored In water, it contains theobromine calcium and calcium mitrite in a molecular ratio. It is easily soluble in water, but the diluted solutions decompose when Gradually stand as the complex disintegrates again. In the way described the new compound is obtained in a form that can easily be filtered off and lets dry, while in the process of the main patent 548 373 after combining the resulting solution first evaporated and then using a vacuum must be dried in a thin layer. The washing mentioned above Precipitation with alcohol is provided in the event that a completely pure compound should be necessary. There is no need to determine the content of the starting materials, those in view of the fluctuating water content of the latter in the process of the main patent is essential.

Beispiel 35 Teile Calciumnitrit löst man in 5o Teilen Wasser und trägt nun unter gutem Durchrühren 22 Teile Theobromin-Calcium (r5 Teilen wasserfreier Substanz entsprechend) ein. Nach 24stündigem Stehen, wobei zeitweise kräftig durchgerührt wird, preßt man auf der Nutsche die Mutterlauge ab und trocknet darauf auf dem Tonteller. Das pulverförmig gewordene Produkt wird im Soxhletapparat mit Alkohol längere Zeit extrahiert. Der Rückstand stellt die kristallwasserhaltige neue liomplexv ei-bindung vor. Sie enthält, auf Trockensubstanz berechnet,. 75 °1o Theobromin-Calcium und 2,5 % Calciumnitrit.EXAMPLE 35 parts of calcium nitrite are dissolved in 50 parts of water and 22 parts of theobromine calcium (corresponding to 5 parts of anhydrous substance) are then introduced with thorough stirring. After standing for 24 hours, during which time it is vigorously stirred, the mother liquor is pressed off on the suction filter and then dried on the clay plate. The product, which has become powdery, is extracted for a long time in the Soxhlet apparatus with alcohol. The residue represents the new liomplexv ei bond containing water of crystallization. It contains, calculated on dry matter. 75 ° 1o theobromine calcium and 2.5 % calcium nitrite.

Claims (1)

PATENTAN'SPRU CH Verfahren zur Darstellung einer Verbindung aus Theobromin-Calcium und Calciumnitrit, dadurch gekennzeichnet, daß man in Abänderung des Verfahrens gemäß Patent 548 373 hier frisch gefälltes, in Wasser nicht lösliches Theobromin-Calcium in überschüssige konzentrierte Calciumnitritlösung einträgt und das Reaktionsprodukt nach dem Trocknen mit Alkohol vom überschüssigen Calciumnitrit befreit.PATENTAN'SPRU CH Process for the preparation of a compound from theobromine calcium and calcium nitrite, characterized in that in a modification of the method according to patent 548,373 here freshly precipitated, water-insoluble theobromine calcium enters into excess concentrated calcium nitrite solution and the reaction product freed from excess calcium nitrite after drying with alcohol.
DEK120377D 1931-05-13 1931-05-13 Process for the preparation of a compound from theobromine calcium and calcium nitrite Expired DE555002C (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
DEK120377D DE555002C (en) 1931-05-13 1931-05-13 Process for the preparation of a compound from theobromine calcium and calcium nitrite

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DEK120377D DE555002C (en) 1931-05-13 1931-05-13 Process for the preparation of a compound from theobromine calcium and calcium nitrite

Publications (1)

Publication Number Publication Date
DE555002C true DE555002C (en) 1932-07-16

Family

ID=7244578

Family Applications (1)

Application Number Title Priority Date Filing Date
DEK120377D Expired DE555002C (en) 1931-05-13 1931-05-13 Process for the preparation of a compound from theobromine calcium and calcium nitrite

Country Status (1)

Country Link
DE (1) DE555002C (en)

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