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[Read Full Article one. Note now the depth of the solution in the flask, and
> Stainless steel cathode
Graphite anodes (2)
Electrochemical cell used to convert a
propenylbenzene to the corresponding phenylacetone.
12 Studies On The Production OfTMA-
be sure that the required amount of electrode surfaces are in the
solution. I depicted graphite sheet anodes, in Figures 6 and 7, but the
more commonly available graphite rods will work as well.
Now, using alligator-clip wiring, attach one clip to the central
stainless steel cathode, and run it to your DC transformer where it is
connected to the black or negative pole. Another approximately onefoot
long section of alligator-clip wiring is
attached to each of the
graphite anodes; i.e. the
alligator-clip on one end
gets attached to graphite
anode A, while the
alligator-clip on the
opposite end of the wire
gets attached to graphite
anode B. Then remove
some insulation in the
center of the wire, and
make an electric
connection to the
positive and red pole on
the DC transformer.
Next, begin vigorous
magnetic stirring of the solution,
turn on the transformer, and adjust the output of the transformer so
that it is pushing a constant current of about 3.4 amps. All three
of the electrodes should be fizzing away at this point. If one appears
dead, dig the alligator-clip into it to make better contact. Continue
passing electricity until 24,000 coulombs have been passed
through the solution. A coulomb is defined as 1 amp-second, so this
takes about 2 hours at 3.4 amps. The patent states that the temperature
must be kept in the range of 10-306 C, so watch to make sure that
Stainless steel cathode
Graphite anode j - Graphite anode
Side view of electrochemical cell.
Practical LSD Manufacture
doesn't heat up the solution too much. Surround the beaker with ice if
The electrochemical cell makes the following compound, an
When the required amount of current has been passed, turn off the
juice and the stirring, and pour the contents of the beaker into a sep
funnel. Allow it to stand for about Vi hour for the phases to fully
separate. An aqueous phase settles out at the bottom of the sep funnel, in
spite of the fact that water and acetronitrile are miscible. This water
phase contains the NaBr. It should be separated off and saved for reuse.
The acetonitrile phase contains the product. It should be poured
into a distilling flask, and the solvent removed under a vacuum. By
packing the receiving flask in dry ice during this process, the
acetonitrile can be recovered for reuse.
The residue of epoxide product left in the flask should be diluted
with 150 ml of ethyl acetate, and poured into a 500 ml flask. Flush the
flask with nitrogen, then add 1.5 grams lithium iodide, and reflux for 5
hours. The lithium iodide catalytically transforms the epoxide to the
After the 5 hours of reflux are over, allow the mixt
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