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Posts 1 - 17 of 17

 Subject: P2P synths 

 

 

 

 

 

 

zooligan
(Hive Addict)
07-13-01 11:10
No 190411

  

  

P2P synths

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O.K.  After reading through SOMM5 and TSII, I decided that of the synths presented, the AlCL3/benzene/chloroacetone synth was the most straightforward and involved the least hard-to-obtain and/or watched chems.

Does anyone know of any other minimal-step synths involving no hard-to-obtain chems?  AB mentioned a toluene/bleach synth, but I never ran across that one (that I remember :P).  There is the reference to the hydratropic aldehyde/H2SO4 ynth in Rhod's section of TSII, but I've never heard any feedback from anyone, positive or negative, on this one.

Let's get some good off-the-radar type P2P synths going ot in the open and get some good alternatives to the birch and rP/I/ephedrine reductions.

z


"And if we don't get some cool rules ourselves, pronto, then we'll just be bogus too!"

 

 

 

 

 

 

lugh
(Hive Bee)
07-13-01 12:50
No 190435

  

  

Re: P2P synths

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Chloroacetone is undoubtedly on many country's watched list, it appears you haven't used the search engine yet, it turned up these posts related to your question going back to March: 36700, 188868, 172438, 180749 Just think how many more you could find if you tried it for yourself, you could learn a lot by using the search engine yourself!
   

 

 

 

 

 

 

Rhodium
(Chief Bee)
07-14-01 11:34
No 190569

  

  

Re: P2P synths

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Zooligan: The toluene/bleach synthesis is one yielding benzyl chloride. I have many unedited posts saved on that method, pm me and I'll email them to you.


http://www.rhodium.ws/

 

 

 

 

 

 

Prdy2GO
(Stranger)
07-16-01 06:58
No 190930

  

  

Re: P2P synths

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SWIM has been through nearly all of the sugested routes In the "Rhodium Section" as training excerizes for the  chilly cookoff. What is your question about them?


Hum did you get that?

 

 

 

 

 

 

goiterjoe
(Hive Bee)
07-16-01 11:04
No 190971

  

  

Re: P2P synths

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you mind mailing those posts to me as well Rhodium?


If pacman influenced us, we'd glide around dark rooms eating pills and listen to repetitive music.

 

 

 

 

 

 

zooligan
(Hive Addict)
07-16-01 11:51
No 190982

  

  

Re: P2P synths

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it appears you haven't used the search engine yet, it turned up these posts related to your question going back to March: 36700, 188868, 172438, 180749 Just think how many more you could find if you tried it for yourself, you could learn a lot by using the search engine yourself!


Hmm... lugh, I will assume that this is your way of answering my question "Does anyone know of any other minimal-step synths involving no hard-to-obtain chems?" as "No."   

"Minimal-step" is the key here, as implied by my mention of the benzene/Al chloride/chloroacetone synth from TSII.  Drip and reflux, then distill out the P2P.  The hydratropic aldehyde synth is also a one-stepper, provided that it actually works.

So has anyone tried any of these synths??  Care to shaare your experiences (successes or failures)?

z


"And if we don't get some cool rules ourselves, pronto, then we'll just be bogus too!"

 

 

 

 

 

 

lugh
(Hive Bee)
07-17-01 08:37
No 191196

  

  

Re: P2P synths

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While this doesn’t provide any chemistry new to the Hive, it does provide some processing details that may be useful:
Phenyl acetic acid possesses a strong, lasting, and somewhat unpleasant sweet odor which becomes honeylike on dilution. Its esters have strong and pleasant odors, the methyl and ethyl having a pronounced honey aroma, the amyl a prune-like note, and the p-cresyl a definite narcissus character. The first three esters are in fairly general use in flavors and perfumes, although only small quantities are needed because of their powerful odor.
Large amounts of phenyl acetic acid were formerly manufactured since it was the main source of phenyl ethyl alcohol. The present production of the acid for perfumery purposes is quite limited. It is inter-esting to note that the salts of the acid are powerful plant hormones and quite possibly may find wide application for this purpose in the future.
The occurrence of phenyl acetic acid or its esters has been reported in a few essential oils. Oil of neroli (Citrus bigaradia R.) is known to contain phenyl acetic acid. It has also been found in Japanese mint oil (Mentha arvensis) [Walbamn, J. prakt. Chem. 2, 96, 248 (1917)] in the form of its hexen-3-ol-1 ester. The probable occurrence of the free acid in tuberose oil (Polyanthus tuberosa L.) has been noted [Hesse, Ber. 36, 1459 (1903)].
Methods of Preparation.-The chemical literature contains numerous reports on the preparation of phenyl acetic acid. The most important method involving the hydrolysis of benzyl cyanide was first reported nearly a century ago and is still widely used for the commercial preparation of this compound. Lewinsohn [Perfumery Essent. Oil Record 14, 336 (1924)] gives the following procedure for manufacturing phenylacetic acid by this method, starting with the readily available benzyl chloride, which is converted to benzyl cyanide and then hydrolyzed to the acid.
Benzyl Cyanide- 6 kilos of potassium cyanide are dissolved in water in an enameled stirring vessel fitted with reflux condenser. There is then added slowly a solution of 10 kilos of benzyl chloride in an equal weight of alcohol. When all has been added, the mixture is heated for three to four hours at the boil. The liquid separates into two layers, the upper one reddish brown, contains the benzyl cyanide, the lower aqueous layer the alcohol and potassium chloride (which is precipitated as a crust on the walls of the vessel on cooling).
The brown oily layer is washed several times with water and then distilled at ordinary pressure. Traces of alcohol first come over and the temperature then rises quickly to 195º C. The residual liquor is now cooled somewhat and the benzyl cyanide distilled off in vacuo without fractiona-tion. The crude benzyl cyanide so obtained is used for the next operation.
Pbenyl acetic acid- In a silica basin of about 35 cm. diameter, a mixture of 2.5 kilos of benzyl cyanide and 7.5 kilos of 70 per cent sulfuric acid is warmed until a few bubbles of gas appear. The heating is at once stopped, since a very vigorous action now ensues. As the vapors evolved are injurious to health, the basin is covered when the reaction begins with a sliding cover from which the vapors can be led into water. As soon as the reaction ceases, the product is poured upon crushed ice in a large, earthenware vessel. Crude phenyl acetic acid, contaminated on the surface with phenyl acetamide, is precipitated on cooling. In order to remove the amide, the acid is dissolved in lukewarm dilute soda solution. The amide remains undissolved and can be filtered off, while the phenyl acetic acid goes into solution as sodium salt and is reprecipitated in a sufficiently pure state by the addition of dilute mineral acid. After drying it is ready for esterification.
Phenyl acetic acid, as well as its ester, is used for the preparation of honey aroma. For this purpose a further purification is necessary. The acid is dissolved in five times its weight of boiling water, filtered off and allowed to cool. Phenyl acetic acid separates out in an absolutely pure state in the form of flakes with a mother of pearl lustre. After filtering and drying it possesses a pleasant honey scent.

 

 

 

 

 

 

terbium
(Hive Addict)
07-17-01 13:20
No 191265

  

  

Re: P2P synths

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The acid is dissolved in five times its weight of boiling water, filtered off and allowed to cool. Phenyl acetic acid separates out in an absolutely pure state in the form of flakes with a mother of pearl lustre. After filtering and drying it possesses a pleasant honey scent.


I used to recrystallize my phenylacetic acid like that but somehow I must not have gotten it as pure as this report since my stuff always still had that funky, definitely not honey, odor. While the odor is not strong most people find it offensive though I got to sort of like it. After working with large quantities of the stuff - filtering, spreading out to dry, turning while drying, packaging; the odor pervades your body, even after changing chlothes and taking a long shower other people can still smell it on you.

 

 

 

 

 

 

cheeseboy
(Hive Bee)
01-25-02 13:21
No 260826

  

  

Re: P2P synths

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So does the hydratropic aldehyde synth work or what?


May The Source Bee With You....Always.

 

 

 

 

 

 

PrimoPyro
(Hive Prodigy)
01-26-02 01:08
No 261052

  

  

Re: P2P synths

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I havent tried it myself, but Id have to say yes it definitely works.

What answer are you looking for? We already said no one here has performed it. If it is on Rhodium's page, it is at least thought to work and there is literature evidence of success. What more do want to hear?

Why dont you try it and tell us what happens?

                                                    PrimoPyro


Vivent Longtemps la Ruche!

 

 

 

 

 

 

PolytheneSam
(Master Searcher)
01-26-02 09:38
No 261138

  

  

Re: P2P synths

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Its in the article.  Post No 201382


http://www.geocities.com/dritte123/PSPF.html

 

 

 

 

 

 

Prdy2GO
(Hive Bee)
01-26-02 10:47
No 261158

  

  

Re: P2P synths

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Hello,
In reference to the post you made below would you please share the unedited notes you were refering to with me?
Most interested in BZCL to P2p and or P2NP--> P2P--->MA
Thank you
"Zooligan: The toluene/bleach synthesis is one yielding benzyl chloride. I have many unedited posts saved on that method, pm me and I'll email them to you."


Don't look at me I didn't do it!

 

 

 

 

 

 

Prdy2GO
(Hive Bee)
01-30-02 09:25
No 262776

  

  

Re: P2P synths

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Does anyone have any additional notes on this? Could you please send them to me?

thanks

Hello,
In reference to the post you made below would you please share the unedited notes you were refering to with me?
Most interested in BZCL to P2p and or P2NP--> P2P--->MA
Thank you
"Zooligan: The toluene/bleach synthesis is one yielding benzyl chloride. I have many unedited posts saved on that method, pm me and I'll email them to you."


Don't look at me I didn't do it!

 

 

 

 

 

 

cheeseboy
(Hive Bee)
01-30-02 12:11
No 262842

  

  

Re: P2P synths

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Hydratropic Aldehyde seems to be a promising route. Cheese WILL perform this run if cheese can get the aldehyde. $130 kg sounds expensive, yet with a 70% return that's 700gm of P2P. And ToTo Too.


May The Source Bee With You....Always.

 

 

 

 

 

 

PolytheneSam
(Master Searcher)
01-30-02 17:57
No 262986

  

  

Re: P2P synths

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Alpha-methylstyrene might be less suspicious compared to hydratropic aldehyde.  See that Berichte article.


http://www.geocities.com/dritte123/PSPF.html

 

 

 

 

 

 

CheshireHouse
(Hive Bee)
05-27-02 04:50
No 314730

  

  

Re: P2P synths

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long time no see, ppls, been out of the country on extended vacation, good to see all is well in beeland.  server's picked up in speed quite a bit too, nice :)

swim found some hydratropic aldehyde for about 80 for single kg, and will let you know how it works out.  anybody have info on just how suspicious/flagged this stuff is?


jen

knowing is the easy part

 

 

 

 

 

 

CheshireHouse
(Hive Bee)
05-27-02 06:47
No 314757

  

  

Re: P2P synths

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hrm... funny how the post i just made, above, shows up in the thread, but not (at least for me) in the thread list, even after refresh...

heh guess that's what i get for posting from the cheshire house :p


jen

knowing is the easy part

 

 

 

 

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