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Offline happycamper723

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Home Project
« on: April 19, 2012, 08:03:41 PM »
I am attempting to extract Coniine (C8H17N) from the seeds, leaves, and shoots of Conium Maculatum (Poison Hemlock). I found an article on how to do so:

"Dr. J. Schorm, of Vienna, the author of this paper, after remarking that in spite of the increase of the consumption of coniine, the methods hitherto in vogue for preparing it yielded an article which darkened on exposure to the air, and the salts of which crystallized but badly, gives the following method for preparing pure coniine and its salts:
Preparation Of Crude Coniine

A. - 100 kilogrammes of hemlock seed are moistened with hot water, and after swelling up are treated with 4 kilogrammes of sodium carbonate previously dissolved in the requisite quantity of water (caustic alkalies cannot be used). The swollen seed is worked up uniformly with shovels, and then placed in an apparatus of 400 kilogrammes capacity, similar to that used in the distillation of ethereal oils, and charged with steam under a pressure of three atmospheres. Coniine distills over with the steam, the greater part separating out in the receiver as an oily stratum, while a part remains dissolved in the water. The riper the seeds, the greater is the percentage yield of oily coniine, and the sooner is the distillation ended. The distillate is neutralized with hydrochloric acid, and the whole evaporated to a weak sirupy consistence. When cool, this sirup yields successive crops of sal-ammoniac crystals, which latter are removed by shaking up the mass with twice its volume of strong alcohol, and filtering. This filtrate is freed from alcohol by evaporation over a water bath, the approximate quantity of a solution of caustic soda then added, and the whole shaken up with ether. The ethereal solution is then cooled down to a low temperature, whereby it is separated from conhydrine, which, being somewhat difficultly soluble in ether, crystallizes out.

B. - The bruised hemlock seed is treated in a vacuum extractor with water acidulated with acetic acid, and the extract evaporated in vacuo to a sirupy consistence. The sirup is treated with magnesia, and the coniine dissolved out by shaking up with ether.

The B method yields a less percentage of coniine than A, but of a better quality.
Rectification Of The Crude Coniine

The solution of crude coniine in ether obtained by either of the above processes is evaporated over a water bath to remove the ether, mixed with dry potassium carbonate, and then submitted to fractional distillation from an air bath. The portion distilling over at 168° C. to 169° C. is pure coniine, and represents 60 per cent. of the crude coniine.

Coniine thus prepared is a colorless oily liquid, volatile at the ordinary temperature, and has a specific gravity of 0.886. At a temperature of 25°C it absorbs water, which it gives up again upon heating. It is soluble in 90 parts of water. It is not altered by light.

The author has formed a number of salts from coniine thus prepared, and finds them all crystallizable and unaffected by light. - Berichte der deutschen chemischen Gesellschaft. - Chem. and Druggist."

Here are my problems as follows:

-Method A is almost impossible due to it's complexity (if you could tell me how to do this on a low budget and minimal attention span, that would be fantastic)
-Method B is perfect, but I lack a vacuum extractor
-Considering Coniine's famous toxicity, I would probably need extra safety precautions to handle it.
-The Conium Maculatum is growing in my back yard. This is more of a bio question (i'll ask it in bio and organic chemistry, btw) but do I need gloves to handle it?

Offline Arkcon

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Re: Home Project
« Reply #1 on: April 19, 2012, 08:11:20 PM »
Both require an ether extraction step, and that's a little hard to get and work with around the home.  Probably you can search for a different extraction procedure to follow, for some other biological product.  We don't have in depth discussions of toxin production here.

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Offline Borek

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Re: Home Project
« Reply #2 on: April 20, 2012, 03:14:52 AM »
Considering Coniine's famous toxicity, I would probably need extra safety precautions to handle it.

Quote
do I need gloves to handle it?

Good that you think about it, but fact that you have to ask so simple questions clearly shows it is not a thing you should try. Look for some less dangerous substances - like essential oils.
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