Xicori
(Hive Bee)
12-06-03 19:58
No 475049
       PCM synthesis
(Rated as: excellent) 		    

High bees!

SWIM again wants to share some experience regarding phenylcyclidine synthesis... todays target molecule is PCM (4-(1-phenylcyclohexyl)morpholine. It is ~10% of PCP´s potency.

The synthesis was based on ../rhodium/clandestine/pcp/, but some changes were made:

1) No distillation of the enamine.
2) Distillation of the PCM freebase under high vacuum.
3) Creating the hydrochloride salt via aq HCl/IPA/Et2O instead of gassing.

so here we go:

Step#1: Formation of the enamine

0,2 mol of Morpholine (17,4ml), 0,2mol of cyclohexanone (20,7ml) and 50ml of Toluene together with 0,3g of p-Toluene sulfonic acid were refluxed with a dean stark trap until no more water seperated (5 hours).


During the reaction the colour changed from white to a slight yellow. - heres the reaction mixture after 5 hours of reflux.

Step #2: removing water from p-TSA monohydrate
0,2 moles of p-Toluene sulfonic acid monohydrate in 70ml of toluene were also heated under a dean stark trap until waterfree. (~3 hours)

Step #3: phenylmagnesium bromide
A Grignard reagent was prepared from 0,21 mol of Bromobenzene and 0,21 mol of magnesium turnings. Diethylether was used as solvent.

Step #4: The enamine from step 1 was cooled in an ice bath, and salted with the anhydrous p-TSA from step 2. (formation of thick white slurry)

Step #5: To this slurry (still in the ice bath) the grignard reagent (prepared in step 3) was added dropwise. After finishes addition the ice bath was removed, and the mixture was stirred for another 40min.

The mixture was poured onto 150ml of ice cubes, 40g of NH4Cl and 40ml of 25% NH4OH.

The phases were seperated, the aqueus phase was extracted once more with Et2O. The organic phases were combined and the solvent removed (athmospheric distillation).

The dark coloured residue was distilled @ ~1,5 torr. At ~70-80°C a small fraction collected (byproducts). The second fraction was collected between 95-120°C (PCM freebase).

micro-distillation apparatus.

gauge for high vacuum

freebase (on the left) in the receiver. The center flask contains the lower boiling fraction (byproducts)

Edwards E2M2 rotary vane pump

The freebase which weighted 15,5g was dissolved in 40ml of Isopropanole (the freebase was not very soluble in the alcohol), and 37% HCl was added until the solution was slightly acidic (the solution warmed up when the acid was added).
Then the PCM.HCl was precipiated using 250ml of Et2O. The product was filtered and washed with some Et2O. After drying it had a weight of 14,5g.

product precipiated after addition of Et2O

some freebase that was still in the distillation apparatus crystallised into very hard chunks.


Because of a relatively strong chemical smell the PCM.HCl was recrystallized from 35ml of Isopropanole to yeild 11,3g of absolutely white PCM.HCl (20% overall yeild)

For details on each reaction step see ../rhodium/clandestine/pcp/

Discussion:

 1) Distillation of the enamine isnt really necessary, but the yeild could be higher if it would be distilled before further usage.

2) Some byproducts are formed (for example condensation of the grignard reagent with unreacted cyclohexanone -> 1-Phenylcyclohexanole) -> This makes a good reaction workup necessary.
Some chemists only evaporate their solvents after the grignard reaction to yeild their end product. - Thats no good laboratory practice...

3) The overall yeild is a bit on the low side, has anybee some ideas how to improve the yeild. (longer reaction times, etc ?)

Thats it so far cool

Best wishes & bee safe!
xicori 		 
 
 
 
    Chimimanie
(Hive Bee)
12-06-03 21:57
No 475064
       Good work!     

Good work Xicori!

Do you care to give a bioassay of such compound?

Duration? How does it compare with straight PCP in term of effects? Also dosage: 40-60mg?... 		 
 
 
 
    pHarmacist
(pHantasticant)
12-06-03 23:04
No 475076
       wow     

Xicori, you do it again!

It is a very, very good idea to post pictures like you do, a writeup with pics reveals so much more than without, but of course you already know that... I'm just like Chimi also very interested in what you would have to say about the character (duration, potency, ect) of this compound.

Great!
(¯`·.¸(¯`·.¸ http://www.bassdrive.com/BassDrive.m3u ¸¸.·´¯)¸.·´¯) 		 
 
 
 
    Xicori
(Hive Bee)
12-07-03 03:41
No 475116
       thanks for the flowers :-D details on bioassay     

thanks for the flowers laugh

details on bioassay follows in a few days... SWIM has a lot to to and had no time to test the substance excessively...

I´ve tried 40mg orally - onset 30min after ingestion... the effect was definitely noticeable (like a very small dose of PCP), but the duration was much shorter... after 3-4 hours swim felt completely back to reality  wink

...next time i´ll try 65 or 75mg orally...

The substance also evaporates very fast when heated on a aluminia foil - so smoking is also one thing to test soon..

have a nice sunday! cool

xicori 		 
 
 
 
    MDMA_AcTIvEsTS
(Stranger)
12-11-03 03:27
No 476038
       RHODIUM:     

RHODIUM:

can you put this in the homepage' Rhodium..." This is another worthy contribution to the hive"

Nice post..wink
MDMA_ActIVeSTs: for the support and prolongation of MDMA'