DE490416C - Process for the preparation of diiodine substitution products of 2-oxypyridine and its derivatives - Google Patents

Process for the preparation of diiodine substitution products of 2-oxypyridine and its derivatives

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Publication number
DE490416C
DE490416C DEC39597D DEC0039597D DE490416C DE 490416 C DE490416 C DE 490416C DE C39597 D DEC39597 D DE C39597D DE C0039597 D DEC0039597 D DE C0039597D DE 490416 C DE490416 C DE 490416C
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DE
Germany
Prior art keywords
oxypyridine
diiodine
derivatives
preparation
substitution products
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
DEC39597D
Other languages
German (de)
Inventor
Dr Max Dohrn
Dr Ralph Dirksen
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.)
Schering Kahlbaum AG
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Schering Kahlbaum AG
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 Schering Kahlbaum AG filed Critical Schering Kahlbaum AG
Priority to DEC39597D priority Critical patent/DE490416C/en
Application granted granted Critical
Publication of DE490416C publication Critical patent/DE490416C/en
Expired legal-status Critical Current

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Description

Verfahren zur Darstellung von Dijodsubstitutionsprodukten des 2-Oxypyridins und seiner Derivate Die Jodierung des 2 - Oxypyridins geht äußerst schwer vonstatten. Beim Behandeln von 2-Oxypyridin mit Jod in Gegenwart von 3 oprozentiger Wasserstoffsup eroxydlösung und etwas Eisen bei erhöhter Temperatur erhält man nur geringe Mengen des 5-Jod-z-Oxypyridins (vgl. Berichte 58 [1925], S. 116).Process for the preparation of diiodine substitution products of 2-oxypyridine and its derivatives The iodination of 2 - oxypyridine is extremely difficult. When treating 2-oxypyridine with iodine in the presence of 3% hydrogen sup Oxide solution and a little iron at elevated temperature are only obtained in small quantities of 5-iodine-z-oxypyridine (cf. reports 58 [1925], p. 116).

Es wurde nun gefunden, daß man mit Hilfe von Chlorjod das 2-Oxypyridin oder dessen Dürivatie in mineralsaurer Lösung leicht in Dijodsubstitutionsprodukte überführen kann.It has now been found that 2-oxypyridine can be obtained with the aid of chlorine iodine or its Dürivatie in mineral acid solution easily into diiodine substitution products can convict.

Beispiel i Zog 2-Oxypyridin werden in 25 ccm verdünnter Salzsäure gelöst und mit 35 g Jodmonochlorid in verdünnter Salzsäure versetzt. Nach mehrstündigem Stehen bei: gewöhnlicher Temperatur scheidet sich das 2-Oxy-3, 5-dijodpyridin in reiner Form ab.Example i 2-Oxypyridine is dissolved in 25 cc of dilute hydrochloric acid dissolved and mixed with 35 g of iodine monochloride in dilute hydrochloric acid. After several hours Standing at: ordinary temperature, the 2-oxy-3, 5-diiodopyridine separates into pure form.

Das z-Oxy-3, 5-dijodpyridin läßt sich aus einem Alkohol-Pyridin-Gemis.ch oder aus Eisessig umkristallisieren. Es schmilzt bei a55°, bei z65° zersetzt ,es sich. In heißer Natronlauge ist es löslich, beim Erkalten kristallisiert die Natriumverbindung aus.The z-Oxy-3, 5-diiodopyridine can be obtained from an alcohol-pyridine-Gemis.ch or recrystallize from glacial acetic acid. It melts at a55 °, decomposes at z65 °, it themselves. It is soluble in hot sodium hydroxide solution; when it cools, the sodium compound crystallizes the end.

Beispiel 2 i o g 2 - Oxy - 6 - methylpyridin werden in 5o.ccm verdünnter Salzsäure mit 309 jo(dmonochlorid in 6o ccm verdünnter Salzsäure vermischt und bei Zimmertemperatur in verschlossener Flasche sich selbst überlassen. Nach ,18 Stunden hat sich das 2 - Oxy-3, 5-dijod-6-methylpyridin als graues Pulver am Boden der Flasche abgesetzt. Man saugt ab, löst in Natronlauge und fällt mit schwefliger Säure. Das rein weiße z-Oxy-3, 5-dijod-6-methylpyridin kann dann noch aus Alkohol umkristallisiert werden. Es schmilzt bei 23o° unter Zersetzung.Example 2 Two-oxy-6-methylpyridine are mixed in 50% of dilute hydrochloric acid with 309 % of monochloride in 60 cc of dilute hydrochloric acid and left to stand in a sealed bottle at room temperature. After 18 hours, the 2-oxy-3 5-diiodo-6-methylpyridine deposited as a gray powder at the bottom of the bottle. It is suctioned off, dissolved in sodium hydroxide solution and precipitated with sulphurous acid. The pure white z-oxy-3, 5-diiodo-6-methylpyridine can then still precipitate Recrystallized alcohol, which melts at 230 ° with decomposition.

Claims (1)

PATENTANSPRUCH Verfahren zur Darstellung von Dijodsubstitutionsprodukten des z-Oxypyridins und seiner Derivate, dadurch gekennzeichnet, daß man 2-Oxypyridin oder dessen Derivate mit Chlorjod in mineralsaurer Lösung behandelt.PATENT CLAIM Process for the preparation of diiodine substitution products of z-oxypyridine and its derivatives, characterized in that 2-oxypyridine or its derivatives treated with chloroiodine in a mineral acid solution.
DEC39597D 1927-04-01 1927-04-01 Process for the preparation of diiodine substitution products of 2-oxypyridine and its derivatives Expired DE490416C (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
DEC39597D DE490416C (en) 1927-04-01 1927-04-01 Process for the preparation of diiodine substitution products of 2-oxypyridine and its derivatives

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DEC39597D DE490416C (en) 1927-04-01 1927-04-01 Process for the preparation of diiodine substitution products of 2-oxypyridine and its derivatives

Publications (1)

Publication Number Publication Date
DE490416C true DE490416C (en) 1930-01-27

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Family Applications (1)

Application Number Title Priority Date Filing Date
DEC39597D Expired DE490416C (en) 1927-04-01 1927-04-01 Process for the preparation of diiodine substitution products of 2-oxypyridine and its derivatives

Country Status (1)

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DE (1) DE490416C (en)

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