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Topic: Method for Free-basing of Amine hydrochloride zink salt  (Read 3820 times)

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Offline Raven

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Method for Free-basing of Amine hydrochloride zink salt
« 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
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Offline rolnor

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Re: Method for Free-basing of Amine hydrochloride zink salt
« Reply #1 on: July 14, 2022, 07:02:08 PM »
Try ether
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Offline Raven

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Re: Method for Free-basing of Amine hydrochloride zink salt
« Reply #2 on: July 15, 2022, 04:13:08 AM »

Thanks rolnor

Ether is no go in large quantities, due to explosion risk and peroxide formation.
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Offline rolnor

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Re: Method for Free-basing of Amine hydrochloride zink salt
« Reply #3 on: July 16, 2022, 07:37:39 AM »
Toluene? What scale is it and whats the structure of the free base?
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Offline Raven

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Re: Method for Free-basing of Amine hydrochloride zink salt
« Reply #4 on: July 16, 2022, 11:04:53 AM »
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Offline rolnor

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Re: Method for Free-basing of Amine hydrochloride zink salt
« Reply #5 on: July 17, 2022, 11:55:05 AM »
That must be highly crystaline? Can you not crash it out and collect on a filter?
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Offline rolnor

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Re: Method for Free-basing of Amine hydrochloride zink salt
« Reply #6 on: July 18, 2022, 03:38:12 AM »
You can dissolve zinc and chloride with warm sodium hydroxide, then the base will crash out.
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Offline Raven

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Re: Method for Free-basing of Amine hydrochloride zink salt
« Reply #7 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:
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Offline rolnor

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Re: Method for Free-basing of Amine hydrochloride zink salt
« Reply #8 on: July 19, 2022, 07:40:07 AM »
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