Author Topic: TCP Synthesis  (Read 2637 times)

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Xicori

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TCP Synthesis
« on: January 26, 2004, 04:00:00 PM »
High Bees!

The time has come to provide you with another chapter of the  Phenylcyclidine derivate synthesis adventure  ;)  Todays target object: TCP













Molecule:

TCP (" C1CCCN(C1)C2(CCCCC2)c3sccc3 ")




Step 1: 2-Thiophene-magnesium bromide

To a 250ml RBF were added 5g (~0,2 mol) of Mg, a crystal of iodine and 50 ml of Et2O. The apparatus was protected from moisture, and 19,1 ml (0,2 mol) of 2-Bromothiophene in 20ml Et2O were added dropwise with stirring until the grignard reaction startet. The Bromothiophene was added dropwise during one hour, and after finished addition the mixture was heated to reflux temperature for further 3 hours.

Here are a few pictures how it looks like when a grignard reaction starts:


The ether is coloured by the iodine. The first drops of bromothiophene have been added.


t+ 20 sec. The colour of the iodine disappears, and the ether gets cloudy.


t+ 35 sec. The mixture starts to boil.


t+ 45 sec. Reaction at full blast. grignards are very exothermic. Apply a cold water bath if the reflux becomes to violent!

There´s a lot of info about grignard rnx here at the hive, so UTFSE for details!

Step 2: Salting on the Enamine with anhydrous p-Toluene sulfonic acid

32g (0,194 mol) of 1-cyclohexenyl-piperidine (for the preperation of the enamine see

Post 451447

(Xicori: "PCP via enamine intermediate [pictures]", Methods Discourse)
) in 80ml of Ether was cooled in an ice bath and dropwise treated with an equimolar amount of anhydrous p-Toluene sulfonic acid in 80ml of Toluene.

Step 3: TCP

To the well stirred & cooled slurry formed in Step 2 was added the grignard solution (Step 1) dropwise. After everything has been added the ice bath was removed and the mixture was stirred for additional 45 minutes.


The grignard solution is added dropwise to the slurry from step 2. Note that all moisture must be excluded!


The mixture after finished addition.

The reaction mixture was poured onto 200ml of crushed ice, and 50g of NH4Cl and 40ml of concentrated aq. ammonia was added. after some minutes of stirring every solid dissolved and the phases were seperated. The aqueous layer was extracted once more with 100ml of Ether, and then discarded. The combined organic phases were washed twice with 100ml of water and dried over sodium sulfate.


The 2 phases in the sep funnel.

Flask: Combined organic extracts with sodium sulfate added. Beaker: aqueous phase - it can be discarded.

The solvent was removed on the rotary evaporator (Ether at 760mm Hg, Toluene at aspirator vakuum ->solvents can be dried and reused!), and the residue was distilled at 1,5mm Hg.


The residue after removal of the solvents.


High vacuum distillation setup


Freebase in the receiver.

The first fraction consisted of a few drops unreacted 2-Bromothiophene, and the second fraction (TCP freebase) which was collected between 120-140°C @ 1,5mmHg weighted 24,2g.

The freebase oil was dissolved in 40ml of IPA and 8ml of concentrated HCl was added dropwise what was very exothermic. Then 300ml of anhydrous ether was added.

The beaker was placed in the freezer for 30min and was the filtered to yield 22g (~40%, based on the amount of enamine used) of white TCP Hydrochloride. 8)


Product drying in a crystallisation dish.


Bioassay: At SWIMs first try the substance gave him a very good impression. It seems to be more potent than PCP, and also the duration seems to be longer. The main effects are basically the same then with PCP, but the TCP seems to be a bit more colorful ;)

That was SWIMs first experience with TCP, so he hopes that he will be able to give more bioassay information during the next weeks!

Enjoy, and bee safe!  8)
Xicori

MDMA_AcTIvEsTS

  • Guest
NICE WORK:
« Reply #1 on: January 27, 2004, 04:05:00 AM »
NICE WORK gota love pics they really do it for me"

keep it up"... :P  :P

SpicyBrown

  • Guest
Excellent!
« Reply #2 on: January 27, 2004, 06:35:00 AM »
Excellent! Absolutely excellent! Congrats on the successful run, you make SWIM jealous! Have yet to try PCP or any of its analogs. Look forward to your more detailed bioassay  ;D

-SpicyBrown

Xicori

  • Guest
Bioassay
« Reply #3 on: February 06, 2004, 05:54:00 PM »
High Bees!

Since the synthesis some bioassay data was collected  8)

Swims motivation in synthing PCP-analogues was to find a substance that actions can be closely compared to ketamine. Ketamine (i.m.) was the drug swim had the nicest experiences with, but it isnt any more available to swim  :( .

So swim hoped to find a pcp analogue which is a good ketamine substitute, and TCP seems to be the compound that is nearly as visionary as ketamine.

If Ketamine (100%) is set as standard for the dissiociative and visionary effects, i would classify the other PCP analogues as follow:

PCP: ~40-50%
TCP: ~70-85%
PCM: ~ hardly 5% (may change with very high dosages >100mg)

It is clear the the dose is also an important factor, but no PCP experience i had yet was comparable to the quality of the TCP trips.


Subject A:
Ingestion form: snorted

I was sitting in front of my computer, chatting with some peaole and decided to try a small amount of TCP. ~2-3mg were snorted and after 3-4min the effects started to kick in. Reading became very hard because the monitor always "faded away". The analgetic effect was very strong, and body coordination became harder and harder (robot-feeling). The plateau was reached within 10-15min, and i spent the time with smoking cigarettes and listening to music (a music tip for dissiociative-freaks: Anima Sound System and Shpongle). Body feeling was great, something euphoric was also present, and the music was felt very clear & intense.

Then  decided to increase the dosage, and so ~8mg were snorted, together with 1,5mg of bromazepame (to prevent olneys lesion). I was lying in bed, listening to music, and only a small orange light was switched on. The body feeling was very intense, like when some force would move your body around the bed/room - hard to describe. The room lost its edges, and was slightly morphing... One moment later i had the feeling that my bed was flying away...slowly the ceiling came nearer, like when the bed would have liftet about 2 metres. With closed eyes other rooms were seen, and my body was moving (or better flying) around in these rooms...(nearly the K-Hole  8) )

I enjoyed the visuals, and after ~3-4 hours the main effects were over, but the afterglow prevented me from sleeping. After some more hours i finally fount sleep to awake very relaxed & without after effects on the next day. All in one a very pleasent and interesting experience.


Subject B tried the substance intramuscularly, with also very nice results. - The report will be written/postet soon.

best wishes,
xicori

whatever

  • Guest
hmmmm...
« Reply #4 on: February 16, 2004, 02:07:00 PM »
Well is ten daze long enough to be way past 'soon'? Very interested in hearing about the IM report. Ketamine via IM versus nasal administration give 'very' different subjective effects. Or so I've been told. Would be very interested in hearing about any subtle differences with TCP via various methods of administration.

chemotype

  • Guest
Fascinating. This bee can't go back down that...
« Reply #5 on: February 24, 2004, 02:01:00 AM »
Fascinating.  This bee can't go back down that path again but this is all quite interesting.  PCPy is an interesting compound also.  A little less potent that PCP. 

bless...

Xicori

  • Guest
Re: Well is ten daze long enough to be way...
« Reply #6 on: February 24, 2004, 02:54:00 PM »


Well is ten daze long enough to be way past 'soon'?




for sure not, but it doent depend on me ´when i finally get this experience report... If u cant awaite the information you should go to all the trouble making & testing the substance!

regards,
x