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