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Chemistry Forums for Students => Organic Chemistry Forum => Organic Chemistry Forum for Graduate Students and Professionals => Topic started by: Raven on July 14, 2022, 05:04:30 PM

Title: Method for Free-basing of Amine hydrochloride zink salt
Post by: Raven on July 14, 2022, 05:04:30 PM
Hello,

I need to free-base a large quantities ( 1-2 kg) of an amine hydrochloride zinksalt. Can someone recommend a method. 
The usual basification and extraction with DMC, is not suitable, due to the that some of the zinc is extracted into the DMC.

Thanks
Title: Re: Method for Free-basing of Amine hydrochloride zink salt
Post by: rolnor on July 14, 2022, 07:02:08 PM
Try ether
Title: Re: Method for Free-basing of Amine hydrochloride zink salt
Post by: Raven on July 15, 2022, 04:13:08 AM

Thanks rolnor

Ether is no go in large quantities, due to explosion risk and peroxide formation.
Title: Re: Method for Free-basing of Amine hydrochloride zink salt
Post by: rolnor on July 16, 2022, 07:37:39 AM
Toluene? What scale is it and whats the structure of the free base?
Title: Re: Method for Free-basing of Amine hydrochloride zink salt
Post by: Raven on July 16, 2022, 11:04:53 AM
Scale: 1-2 kg

http://www.chemspider.com/Chemical-Structure.56136.html?rid=ba6106c9-b743-4b4c-aade-bb0ddc91e868&page_num=0 (http://www.chemspider.com/Chemical-Structure.56136.html?rid=ba6106c9-b743-4b4c-aade-bb0ddc91e868&page_num=0)
Title: Re: Method for Free-basing of Amine hydrochloride zink salt
Post by: rolnor on July 17, 2022, 11:55:05 AM
That must be highly crystaline? Can you not crash it out and collect on a filter?
Title: Re: Method for Free-basing of Amine hydrochloride zink salt
Post by: rolnor on July 18, 2022, 03:38:12 AM
You can dissolve zinc and chloride with warm sodium hydroxide, then the base will crash out.
Title: Re: Method for Free-basing of Amine hydrochloride zink salt
Post by: Raven on July 19, 2022, 03:45:29 AM
How do I prevent the formed Zn(OH)2 to crash out?
Zn2+ +2OH-  :rarrow: Zn(OH)2 :spindown:
Title: Re: Method for Free-basing of Amine hydrochloride zink salt
Post by: rolnor on July 19, 2022, 07:40:07 AM
It will form sodium zincate.

https://en.wikipedia.org/wiki/Sodium_zincate