DE551145C - Process for the preparation of iodomethanesulfonic acid or its salts - Google Patents

Process for the preparation of iodomethanesulfonic acid or its salts

Info

Publication number
DE551145C
DE551145C DE1930551145D DE551145DD DE551145C DE 551145 C DE551145 C DE 551145C DE 1930551145 D DE1930551145 D DE 1930551145D DE 551145D D DE551145D D DE 551145DD DE 551145 C DE551145 C DE 551145C
Authority
DE
Germany
Prior art keywords
salts
acid
preparation
iodomethanesulfonic
sodium
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
DE1930551145D
Other languages
German (de)
Inventor
Dr Gerhard Hecht
Dr Anton Ossenbeck
Dr Ernst Tietze
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.)
I G FARBEINDUSTRIE AKT GES
Original Assignee
I G FARBEINDUSTRIE AKT GES
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 I G FARBEINDUSTRIE AKT GES filed Critical I G FARBEINDUSTRIE AKT GES
Application granted granted Critical
Publication of DE551145C publication Critical patent/DE551145C/en
Expired legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
    • C07C303/02—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof
    • C07C303/22—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof from sulfonic acids, by reactions not involving the formation of sulfo or halosulfonyl groups; from sulfonic halides by reactions not involving the formation of halosulfonyl groups

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)

Description

Verfahren zur Darstellung von Jodmethansulfonsäure bzw. ihren Salzen Durch das Patent 532 766 wird ein Verfahren zur Darstellung der jodmethansulfonsäure bzw. ihrer Salze geschützt. Es besteht darin, daß man Methylenjodid mit neutralen, zweckmäßig wasserlöslichen Sulfiten umsetzt und das Reaktionsprodukt gegebenenfalls in andere Salze überführt. Bei der Weiterverfolgung dieses Arbeitsgebiets wurde nun gefunden, daß man die jodmethansulfonsäure bzw. ihre Salze vorteilhaft auch in der Weise darstellen kann, daß man chlormethansulfonsaure Salze mit Alkali- oder Erdalkalijodiden in Wasseroder organischen Lösungsmitteln auf höhere Temperatur- erhitzt. Beispiel i 152,5 Gewichtsteile chlormethansulfonsaures Natrium werden in 305 Gewichtsteilen Wasser gelöst, mit i 5o Gewichtsteilen wasserfreiem Natriumjodid versetzt und 2o Stunden in geschlossenem Gefäß auf etwa igo° erhitzt. Hierauf wird die Reaktionsmasse zur Trockne verdampft und aus dem Rückstand das gebildete jodmethansulfonsaure Natrium mit Methylalkohol ausgezogen. Es ist identisch mit dem nach Beispiel i des Patents 532 766 erhaltenen jodmethansulfonsauren Natrium. An Stelle des Wassers kann man auch organische Lösungsmittel, wie z. B. Alkohol, verwenden. Beispiele 15 Gewichtsteile chlormethansulfonsaures Natrium und 15 Gewichtsteile Natriumjodid werden in 3o Gewichtsteilen Äthylenglykol i o Stunden ,auf i 9o bis 2oo° erhitzt, wobei nach anfänglicher Lösung allmählich Ausscheidung von N.atriumchlorid eintritt. Hiernach läßt man erkalten, versetzt den Kristallbrei mit Aoeton, saugt ab und kristallisiert das zurückbleibende jodmethansulfonsaure Natrium aus Methylalkohol um.Process for the preparation of iodomethanesulphonic acid or its salts Patent 532 766 protects a process for the preparation of iodomethanesulphonic acid or its salts. It consists in reacting methylene iodide with neutral, suitably water-soluble sulfites and converting the reaction product into other salts, if necessary. In pursuing this field of work, it has now been found that iodomethanesulfonic acid or its salts can advantageously also be prepared by heating chloromethanesulfonic acid salts with alkali or alkaline earth metal iodides in water or organic solvents to a higher temperature. Example i 152.5 parts by weight of sodium chloromethanesulfonate are dissolved in 305 parts by weight of water, i 50 parts by weight of anhydrous sodium iodide are added and the mixture is heated to about igo ° for 20 hours in a closed vessel. The reaction mass is then evaporated to dryness and the sodium iodomethanesulfonic acid formed is extracted from the residue with methyl alcohol. It is identical to the sodium iodomethanesulfonate obtained according to example i of patent 532,766. Instead of water, you can also use organic solvents, such as. B. alcohol, use. EXAMPLES 1 5 parts by weight of sodium chloromethanesulfonate and 15 parts by weight of sodium iodide are heated to between 90 and 200 ° in 30 parts by weight of ethylene glycol for 10 hours, with sodium chloride gradually separating out after the initial solution. It is then allowed to cool, the crystal pulp is mixed with aoeton, filtered off with suction and the remaining sodium iodomethanesulfonic acid is recrystallized from methyl alcohol.

Beispiel 3 1/#. Mol Calciumjodid und i Mol chlormethansulfonsaures Calcium werden, in 6oo ccm Wasser gelöst, wie in Beispiel i zur Reaktion gebracht. Die Reaktionsmischung wird nach Beendigung der Reaktion in gleicher Weise wie in Beispiel i .aufgearbeitet. Das so erhältliche Calciumsalz kann durch Ansäuern mit Schwefelsäure in bekannter Weise in die freie jodmethansulfonsäure umgewandelt werden.Example 3 1 / #. Mole of calcium iodide and 1 mole of chloromethanesulfonic acid Calcium are dissolved in 600 ccm of water, as in Example i, reacted. After the reaction has ended, the reaction mixture is prepared in the same manner as in Example i. Worked up. The calcium salt thus obtainable can be acidified with Sulfuric acid can be converted into the free iodomethanesulfonic acid in a known manner.

Claims (1)

PATENTANSPRUCH: Abänderung des durch Patent 532,766 geschützten Verfahrens zur Darstellung von jodmethansulfonsäure bzw. ihren Salzen, dadurch gekennzeichnet, daß man chlormethansulfonsaure Salze mit Alkali-oder Erdalkalijodiden in Wasser oder einem organischen Lösungsmittel auf höhere Temperatur erhitzt.PATENT CLAIM: Modification of the process protected by patent 532,766 for the preparation of iodomethanesulphonic acid or its salts, characterized in that chloromethanesulphonic acid salts with alkali or alkaline earth iodides in water or an organic solvent are heated to a higher temperature.
DE1930551145D 1930-05-04 1930-05-04 Process for the preparation of iodomethanesulfonic acid or its salts Expired DE551145C (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DE551145T 1930-05-04

Publications (1)

Publication Number Publication Date
DE551145C true DE551145C (en) 1932-05-31

Family

ID=6562936

Family Applications (1)

Application Number Title Priority Date Filing Date
DE1930551145D Expired DE551145C (en) 1930-05-04 1930-05-04 Process for the preparation of iodomethanesulfonic acid or its salts

Country Status (1)

Country Link
DE (1) DE551145C (en)

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