Author Topic: PCP ''bucket'' (Maddox) method: questions.  (Read 123 times)

hyjroul

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PCP ''bucket'' (Maddox) method: questions.
« on: April 23, 2012, 08:08:40 PM »
Hey, a friend will be dreaming on that, procedure he will use hypotetically speaking, note the ghetto style:

Bucket A (10liter plastic bucket with lid); mix well:

198g sodium metabisulfite
200g cyclohexanone

Bucket B (10 liter plastic bucket with lid) mix well :

190g. NaCN (Sodium cyanide)
230g. Piperidine

Add bucket A to bucket B, remove a lot (15minutes more less) and then allow to stand with lid for one day.

PCC is formed as a semicrystalline or crystalline cake on top of the aqueous layer ; removal on PCP and allow to dry.

Bucket C (10 liter plastic bucket with lid and a trash bag) mix well:

74g magnesium (Mg) metal turnings
475g bromobenzene
2 iodine crystals

when baggie blows up because of exothermic reaction , add 1,5L  of dry diethylether and another 25g of bromobenzene , mix well.

Disolve 150g of PCC (piperidincyclohexancarbonitrile) in 1,5L hexane and add to bucket C with the grignard reactive (phenylmagnesium bromide in ether), stir a lot with a large plastic stick (15 mins) and filter the cyanide , add more hexane (500mL), stir, and gassify with HCl gas (from H2SO4 + NaCl with a drying CaCl2 tube) , filter the PCP HCl crystals.

Gassify until no more PCP crystals , combine filtrations and add 1/3 cup of NaOH crystals , 3/4 pints of ethyl ether and 4/4 pints of distilled water (dH2O) , stir and cover, decant ether layer for PCP freebase dissolved in ether, repeat until all dissolved.

Save the top layer.

Enjoy!!

QUESTIONS:

Are this quantities enough for carrying the reaction at such circumpstances with success? Are there any step that can be omitted or I need to add any extra step??

Is there the possibility of high concentrations of deadly HCN gas and possibility of serious intoxication  if done EXACTLY this way?

Are quantities of solvents enough??

What do you will improve of this procedure?

What are approximate yield of this synth and if done this way what are the chances of getting a relatively pure product (PCP freebase, with little PCC contamination, for example 75%+) and in good yield?

Thank you a lot in advance community!!

Vesp

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Re: PCP ''bucket'' (Maddox) method: questions.
« Reply #1 on: April 23, 2012, 08:46:43 PM »
This is such an awful procedure and post/thread I am really not sure what to do with it.

Obviously you are new to this, and I used to be like that (kinda) --  so I can understand where you are coming from, however I really feel you HAVE NOT done enough research into this and are simply trying to be spoon fed by posting a procedure probably taken off of anarchist cookbook.

This (as well as your last thread) did not follow the rules of The Vespiary either. So I am going to lock & toss this thread, but also suggest you research out the reactions, step by step, and try to understand the mechanisms involved in each step, and each reaction, etc...  A lot of these steps will probably result in a fire-y explosion and poisonous material spilling all over hell, resulting in a pay raise for a journalist.

Also here are some good red flags that your procedure is a "bit" sketchy.
1. It suggests using plastic buckets for every step, including the Grignard.
2. Anything that monitors a reaction using an exploding bag is probably a bad thing.
3. Sources! Where the hell did you find this procedure? Do you know if it was a clown that wrote it, or if it has ever been performed by anyone?
4. "Add bucket A to bucket B, remove a lot (15minutes more less) " what does that even mean? Don't follow instructions that do not make sense, especially if you do not understand the reaction that is going on or supposed to happen.

Watch some videos about how the Grignard reaction. Notice any differences in caution taken, quantities, materials used, extra steps, etc?

http://www.youtube.com/watch?v=Raeh26H8S7Y
http://www.youtube.com/watch?v=X70AKnefB-4&feature=related


Notice your colony status if you haven't yet:  +0/-8
Such a score might suggest you are not doing something that is very agreeable among members.
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Vesp

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Re: PCP ''bucket'' (Maddox) method: questions.
« Reply #2 on: April 23, 2012, 10:36:00 PM »
Here is what one member was going to say before I locked this thread:

Quote from: hyjroul

Are this quantities enough for carrying the reaction at such circumpstances with success? Are there any step that can be omitted or I need to add any extra step??

First logical step in your endeaveour would be to actually understand the reactions and calculate the stochiometry being used ::) (See attached image). That way, you'll be able to answer your questions by yourself on this synthesis or any other one. ;)

Quote from: hyjroul

Is there the possibility of high concentrations of deadly HCN gas and possibility of serious intoxication  if done EXACTLY this way?

Fooling around with chemicals that have the possibility to release deadly HCN gas under certains conditions without a clue about which chemicals are incompatible is FUCKING STUPID, RECKLESS AND DANGEROUS. You're only going to smell hydrogen cyanide once  ::). Anyway, keep those cyanides salts away from strong minerals acids like HCl which will release the gas according to this equation:

NaCN(s) + HCl(aq) ---> HCN(g) + NaCl(s)



Note that there might be others conditions under which NaCN can release HCN. That's the only way I remember on top of my head though right now






Are quantities of solvents enough??

What do you will improve of this procedure?

What are approximate yield of this synth and if done this way what are the chances of getting a relatively pure product (PCP freebase, with little PCC contamination, for example 75%+) and in good yield?

Thank you a lot in advance community!!
[/quote]



AND HERE IS THE PICTURE I WANTED TO ATTACH WITH THE CALCULATED STOCHIOMETRY... http://imageshack.us/photo/my-images/215/hyjroul.gif/


Lol @ ''Baggie Blowing'' , ''Bucket Chemistry'' , ''GERNARD reaction'', + other lousy shit in that procedure. I'm wondering how comes they're not having any problem with initiating the Grignard in that bucket though   :o I wouldn't like to be near that shit for sure ROFL. As lugh pointed out, it must smells a lot. Piperidine smells like shit and I assume that what I've smelled from impure PCP was Phenylcyclohexylcarbonitrile, which also smells like shit. Smells more like rotten fish than methylamine  ::)


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