TCP Synthesis

(Rated as: excellent)

High Bees!
The time has come to provide you with another chapter of the Phenylcyclidine derivate synthesis
adventure wink 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!
Theres 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 120-140C @ 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.cool

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! cool
Xicori

Xicori
(Hive Bee)
02-06-04 17:54
No 486907
Bioassay
(Rated as: excellent)
High Bees!

Since the synthesis some bioassay data was collected cool

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 frown.
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 1015min, 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 cool)
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
(Stranger)

02-16-04 14:07
No 489041
hmmmm...
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
(Newbee)
02-24-04 02:01
No 490698
Fascinating. This bee can't go back down that...
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
(Hive Bee)
02-24-04 14:54
No 490796
Re: Well is ten daze long enough to be way...
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