happycamper723
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Coniine!
I have found two methods so far for the extraction of Coniine from poison hemlock (conium maculatum).
The first and probably most trustable:
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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.
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-Dr. J. Schorm
And then the suspicious internet guy (some godforsaken forum):
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Coniine’s extraction from the raw hemlock is carried out by the means of steam-distillation from freshly harvested plant segments and alkalized with
addition of caustic soda or lime prior to distillation.The collected distillate is then cooled, made acidic by careful titration with dilute sulfuric
acid, and the volume of solution is reduced by vacuum evaporation to about a 1/3 - 1/4 of original volume. This concentrated solution is then cooled,
its pH adjusted to 9.5 -10.0 (with 4M NaOH), the solution is further saturated with NaCl, cooled to a T below 10°C and extracted by 5 portions of
ether.The ether extracts are collected and dryed with anhydrous Na2CO3, the ether is then distilled off of a steambath. |
This is all very easy, but I need to use something in place of a vacuum evaporator/extractor.
[Edited on 29-4-2012 by happycamper723]
"Science, eh? Hmmm...I think I read somewhere that science is used to make BOMBS! TERRORIST!!!"
-Homer Simpson
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watson.fawkes
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Neither of these is worthy of anyone else's trust unless you cite your references. What you've done is quotation, not reference.
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happycamper723
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I've edited it. It was an article in the Scientific American by Dr. J. Schorm, from Vienna, from some time ago.
"Science, eh? Hmmm...I think I read somewhere that science is used to make BOMBS! TERRORIST!!!"
-Homer Simpson
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