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Topic: dry HCl in ethyl ether solution without gassing  (Read 4957 times)

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Offline dantax

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dry HCl in ethyl ether solution without gassing
« on: April 24, 2016, 11:22:23 PM »
if adding 20ml of 37% HCl aqueous solution to 80ml of ethyl ether - is it possible for majority of the hydrogen chloride to go into the ether and using sep funnel remove the aqueous layer, resulting in ~37% HCl ethyl ether solution?   or would the HCl want to stay in the aqueous layer?

another idea was to add 20ml 37% HCl aqueous solution into 80ml acetone and use molecular sieves or magnesium sulfate to dry it.

any input appreciated

Offline raylab13

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Re: dry HCl in ethyl ether solution without gassing
« Reply #1 on: April 25, 2016, 12:49:27 AM »
The first plan will absolutely not work. All of the HCl will stay in the aqueous layer.

Molecular sieves might give you a better shot but I'm not quite sure. Good luck!
« Last Edit: April 25, 2016, 01:08:53 AM by raylab13 »

Offline discodermolide

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Re: dry HCl in ethyl ether solution without gassing
« Reply #2 on: April 25, 2016, 02:06:20 AM »
Just bubble HCl gas through ether at 0°C.
I certainly would not use acetone and aqueous HCl.
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Offline Dan

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Re: dry HCl in ethyl ether solution without gassing
« Reply #3 on: April 25, 2016, 02:41:34 AM »
You can also buy dry HCl in diethyl ether or dioxane. This is what I normally do.

Another cylinder-free option is this: http://curlyarrow.blogspot.fr/2009/03/how-to-make-dry-hcl-gas.html
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Offline dantax

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Re: dry HCl in ethyl ether solution without gassing
« Reply #4 on: April 28, 2016, 01:47:21 PM »
thanks everyone thus far for the helpful comments.

At Sigma they sell HCI in ether or dioxane solution, however it is only 2M and 4M solutions and very expensive.

i was really hoping someone might have had experience drying aqueous HCl Acetone solution using molecular sieve or magnesium sulfate.  (i might still try this and report back, main concern was if HCl and magnesium sulfate would react)


I have access to buy the cylinder, however it is sold in too large of a quantity.


It seems like i may have to end up bubbling it, I have almost every piece to make apparatus to gas HCl over calcium chloride - i would prefer to setup a trap,  iam wondering if i should also setup a bubbler with sulfuric acid for the gas to pass through or will calcium chloride eliminate more than 99% of the water upon drip?


ideally i would like to bubble into Acetone rather than Ether due to higher BP.
i need exactly 3.4grams of HCl in my solution, and prefer to use as little solvent as possible (50-100ml or under).

Q: How will i know when i exactly have 3.4grams of HCl in my solution?   i was thinking to do this over a  scale, take weight of flask+solvent with apparatus attachments before and during hcl addition.  (i wont have the receiving flask attached to retort stand)
--> IF there is less than 5% loss during gassing, then i dont need to worry about weighting it, i can just have only 8ml of 37% HCl aqueous solution drip and that would equate to 3.4grams.   
Q: can anyone confirm if loss is minimal?

The HCl/Acetone solution is going to be used in reaction same day. it will not be stored or around any oxidizers.

Offline Babcock_Hall

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Re: dry HCl in ethyl ether solution without gassing
« Reply #5 on: April 28, 2016, 02:43:59 PM »
You can also buy dry HCl in diethyl ether or dioxane. This is what I normally do.

Another cylinder-free option is this: http://curlyarrow.blogspot.fr/2009/03/how-to-make-dry-hcl-gas.html
Dan,

I seem to recall that you or someone else once mentioned making HCl by using methanol and acetyl chloride.  I don't have a recipe handy, however.
EDT
This thread seems pertinent:  http://www.chemicalforums.com/index.php?topic=50618.0
« Last Edit: April 28, 2016, 02:56:52 PM by Babcock_Hall »

Offline Dan

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Re: dry HCl in ethyl ether solution without gassing
« Reply #6 on: April 28, 2016, 03:26:45 PM »
Dantax, acetone may not be a good choice. It condenses with itself under strongly acidic conditions, releasing water. Ethers (including dioxane) are a better options if you need aprotic conditions.

If you can use an alcoholic solvent for your application, solvolysis of AcCl or TMSCl are good options - more convenient and safer than HCl gas.
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Offline zarhym

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Re: dry HCl in ethyl ether solution without gassing
« Reply #7 on: April 29, 2016, 04:33:43 AM »
 we just bubble HCl gas through ether. The conc. of the solution can be determined by the change of the mass.

Offline orgopete

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Re: dry HCl in ethyl ether solution without gassing
« Reply #8 on: April 30, 2016, 10:34:24 AM »
Perhaps you could tell us why you need it and someone might suggest alternate reagents or reactions.
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