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Cleaning up PCP

kakti

kakti

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I originally posted this in Other Drugs, but it just got lost, so I figured maybe the sharper minds here could help me out.

A friend of mine has been getting some yellowish liquid PCP lately, and asked me how to clean it up. Well, I couldn't find any solubility charts, or really much info at all on the properties of phencyclidine (is the freebase a solid or oil?, is the yellow color from impurities or does a solution of the salted form cause the color?) Can anyone recommend a way to clean up and recrystalize a solution of street PCP? And does anyone know how to separate out the PCC that might be left over from the synthesis?
 
or maybe it's just a little bottle of real formadahyde. not phencyclidine at all.

as i recall, the jar with the frog in it in science class sure did look like it was filled with an amber colored fluid...
 
Phencyclidine [77-10-1] Colorless crystals, mp 46-46,5 C, bp 135-137 C.

PCP HCl [956-90-1] mp 233-235 C

PCP HBr mp 214-218

No mention of solubility.

What kind of equipment does he have available? Distillation could be a good way to do some purification depending on what more is in there. But I don't know the synthesis of PCP, so it's just a guess.
 
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Of course, but it may already be a salt in solution, or is PCP usually sold as freebase?
 
From Clarke's

Solubility for the HCl salt:

Soluble 1 in 6 of water, 1 in 7 of ethanol, and 1 in 2 of chloroform; very slightly soluble in ether.




If there's any doubt as to whether or not the substance in question is PCP;

PCP will give a red color with Van Urk reagent upon heating for 3 mins.



Van Urk reagent (Adapted from Clarke's - to be freshly made before use) Dissolve 2.0 g of p–dimethylaminobenzaldehyde in a solution of 50 mL of 95% EtOH & 50 mL of conc HCl
 
if you have access to pdmab, you should be able to tell the difference between chloroform and an amine. if it is a liquid, it is probably the base. unless it is dissolved in something, in which case, evaporate it off. try washing with solvent first, if that doesnt work, then try to recrystalize.
 
What's Clarke's?

The base is solid at room temperature. Apparently there's a lot of gunk in there. Does it smell of solvent? Try to dry it, and if it forms a solid, then recrystallize from ether.
 
It is definitely phencyclidine, from what my friend says it has a very distinct smell that he cannot relate anything else to. Thanks for the solubility and properties info guys, I'll tell him to first evaporate, then go from there.
 
What's Clarke's?
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Sorry, thought everyone around here knew about this

Clarke's Analysis of Drugs and Poisons is available in hardback or online, where a trial registration is offered. If you are serious enough you can D/L a large portion of this book during the trial - I almost got the lot.

Online version is available here. Other books are also hosted.
 
what causes the yellow?

everything i read about PCP weither its on that DEA website or erowid points out that the yellow color is the result of poor manufactureing procedure, they do not specify what the contaminant is, or if it is dangerous. does anybody know what causes this color and if it increases the toxicity of the PCP. What is the most likely contaminant? how pure is most street PCP?
 
If you want, you can stir the oil in an acid like muriatic acid (HCl. and needs to be somewhat concentrated, like at least 0.1 M) and it will make the amine HCl salt in solution (as long as you use just enough to dissolve it, you'll see why). Then you can add ether or a hydrocarbon solvent and shake it, let it separate and decant the organic phase, this should clean it up a bit. Then you need to basify your solution by adding a simple base (NaOH, pure ammonia(nasty) or something like it. Baking soda or NaHCO3 will work). and cool the solution and crystalline PCP should crash out. Be sure to wash the crystals with ice cold water to get rid of the excess aqueous reagents.

Am i wrong? I've never seen much less done experiments with PCP, but from its structure this should work. I don't know its water solubility in cold water as a free base.

This will get rid of any non-amine impurities that are in the oil that are soluble in hydrocarbons, and also get rid of any water-soluble impurities

It's a pretty simple molecule, I don't know the synthesis, but the by-products are probably things like piperidine (it'll extract with the PCP), cycohexanone, and benzene.,,, oh wait, just found the synthesis on erowid.... Yeah, do this extraction, otherwise you might be ingesting cyclohexanone, bromobenzene (BAD) and possibly benzene if they're making the grignard and doing the synth as per in erowid (any water turns a grignard reagent to the hydrocarbon form... basic ochem), and 1-piperidinocyclohexanecarbonitrile that is made from cyanide. Yeah, cyanide, so you definitely want to clean it up until this stuff is pure.
 
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cyclohexanone has a very typical smell, probably traces could be detected in the material
 
^ Absolutely, particularly as PCP is smoked.

Pyrolytic fate of piperidinocyclohexanecarbonitrile, a contaminant of phencyclidine, during smoking.

Authors:

Lue LP
Scimeca JA
Thomas BF
Martin BR

Author Address: Department of Pharmacology and Toxicology, Medical College of Virginia, Virginia Commonwealth University, Richmond 23298-0001.

Source: J Anal Toxicol. 1988 Mar-Apr; 12(2):57-61. [Journal of analytical toxicology]

Abstract:

The pyrolysis products of 1-(1-piperidino)cyclo-hexanecarbonitrile (PCC), the major contaminant of illicit phencyclidine (PCP), have not been previously reported. In order to quantify PCC in mainstream smoke as well as to identify the pyrolysis products, [3H]piperidino-[14C]cyano-PCC was synthesized. Marijuana placebo cigarettes were impregnated with this double-labeled PCC and burned with an apparatus that simulated smoking. The mainstream smoke was passed through a series of traps containing glass wool, H2SO4, or NaOH. Approximately 75% of the 3H was collected in these traps, and 46, 11, and 5% of the 14C was found in the glass wool, H2SO4, and NaOH traps, respectively. Contents of the traps were analyzed by GC/MS. The glass wool trap contained 1-(1-piperidino)-1-cyclo-hexene, PCC, piperidine, and N-acetylpiperidine, and cyanide ion was detected in all three traps. Approximately 47% of the PCC was found intact in mainstream smoke. Approximately 58% was cleaved to form cyanide and 1-(1-piperidino)-1-cyclohexene. The latter was further broken down to cyclohexanone (which represented 21% of the starting material), piperidine (29%), and N-acetylpiperidine (7%), and about 2% remained intact.
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