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12345x
(Stranger)
11-01-02 04:50
No 375355
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there
are other ways
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useing red phos and iodine
or lithium and ammonuia
are widespread and obtaining
these reagents are getting harder
and harder.
for these reasions a differnt route
from phudo to meth will be presented
the basic plan is first to do a
halagenation reaction.using proven
reactions.
then we base the bromoephed gently to remove the positive
proton attached to the amino atom
but gently so as not to cause a reverse reaction of the bromine back to a hydoxy
group.
on the the 2nd step we remove the halogen and replace
it with hydrogen.
we will use a proven, but not comminly used
in this way, method.
1. we make bromoephedrineHCL from phudoHCL or ephedHCL
by using proven bromating agents "ref chem helvena acta 1927"
(PBR5) "phosphorous pentabromide"
or thenyl bromide is mixed with an equal vol of
chloroform or other sutable solvent.
then to this is added phudoHCL in a slightly excess of 1:1 molor ratio in
favor of the bromating reagent.
after a few min.the phudo should have desolved in the
liquid indicating
the conversion to bromoephed has occured.
we now purify the bromeephed by addion of 2x the volume
of our liquid with carbon tetrachloride.
the cristals are filtered and rinced with any NP solvent
we then desolve the cristals in cold water and add cold baking soda water or
other mild base
and extract with ether.
the base bromoephed desolved in ether is added with
anhidress sodium sulfate or any other sutable
drying agent.
in a jar capped,shaken and put aside in the fridge
activated mag turnings (see below for activing mag turning) or freshly cut
mag turnings in a slightly excess moler
ratio of 1:1 to bromoephed. is added to a round bottom 3 neck flask.
dry ether is added just enough to cover the turnings
a condenser is placed on the center neck with a CO2 and water trap (look this
on up ok)
connected to the top of the condenser
and the water jacket lines are hooked up.
the solution in the jar is filtered and the liquid
trasfered to an pressure equalizing sep funnel.
and placed on one of the side necks on the three reaction flask and a cap is
placed on the sep funnel.
the third neck on the flask is connected to an argon
bottle and argon is pumped in to purge the air out of
the flask and condenser.
the neck with the argon is opened and an
iodine crystal is dropped in and pushed to the bottom of the flask with a
glass rod
then after the rod is removed a cap is placed on the neck opening.
with your hand warm the outside of flask in the area where the iodine cristal
is siting.
when bubbles start forming and the iodine purple color disappers."these
are signs the reaction has started"
then crack open the sep funnel and run apx 5% of the funnels volume into the
flask.
if the iodine has truly started the reaction
you should see boiling of the solvent (ether) and the purple color
dissapearing occuring without any ext .heat input.
and within 5 mins .after you droped the iodine crystal in
if not..
add another iodine crystal and try to get it to start boiling with the purple
color disapering.with your hands heat
do not add any more liquid from the sep funnel untill
you have got the flask boiling on its own.
once this has happened
start the water flow thru the water jacket on the condenser wait untill the
reaction peaks then starts slowing down
then open the sep funnel to produce a steady drip
with a rate around 1 drop per sec.
after a few mins.the reaction speed should have stabelized
to the drip rate.
now by watching where on the condenser the ether is turning to liquid
and above that point is dry.
you can increase the drip rate in small incriments.waiting
to see how much higher the liquid condenses up the coloum.
adj the drip rate to the fastest rate that can be had without the very top of
the condenser geting wet
"ie: adj so you have an inch of dry space at the top of the condenser.
when all the liquid has been added shut the sep funnel off
and when the boiling has almost stoped.
apply heat with a heating mantle to keep the boiling for 30 mins longer.
then remove the heating mantle let cool
then set a pan of ice water under the reaction flask .
add in a 2:1 molor ratio dilute HCL "2m" slowly "use the sep
funnel already on the flask"
after the acid has been added.
remove the contents and filter out any mag turnings.
return the contents to the flask set up the condenser
for distilation .
and heat with a mantle untill all the ether has been removed.
remove and discard the ether from the reciver flask
place a clean reciver flask at the end of the distilling coluiom.
add a 50% lye/water solution slowly untill a ph of > 13 is reached to the
reaction flask.
bring up the temp to boiling.
then thru a side neck attach a steam source with a glass tube so the steam
enters at the bottom of the liquid
steam distill untill a test at the end of the condenser shows a ph of
< 8 for at least 5 mins.
remove the contents of the reciver .
add ether and rince and discard the water twice .
dry the meth /ether solvent with sodium sulfate and filter out solids
to some fresh dry ether pump dry HCL gas in untill saturated .
take the acid ether solution and add to the meth ether
solution
stir a few secs.and let sit undesturbed.for 10 mins
decant the liquid and save for extraction with ether/gas
later.
rince your crystals once with fresh dry ether.
and dry.
your done
the theory behind this reaction is to form a grinyerd reagent with the
bromoephed instead of the standerd reagent "bromobenzene"
the result after the contents of the sep funnel is added
is bromo magnesium ephedrine "N,methyl-1-magnesiumbromide
-1-phenyl-2-amino propane"
then instead of using the formed reagent with anouther
compound as is usuly done.
we decompose it with the addtion of acid water.
this results in a hydrogen "from the water "replacing the
(MG-BR) group on the ephed.resulting in meth
and the rest of the water (OH) combining with the (BR-MG)
group forming (BR-MG-OH)
note* to activate old mag turnings
wet them with some dry toluine and pulverize them by whatever means
to break them up to expose fresh "unoxidized mag."
then store them in a air tight jar untill ready to use.
when using dont try to dry the solvent off them as youll
oxadize them in the prossess.just throw them in damp.
the only questionable or easy to screw up , part of this reaction is basing
out
the bromoephed carfuly so as not to turn it back into phudo
thats why we use a weak base instead of lye
and why we base it then store it....
cold .
also make sure everything going into that three neck flask
up untill the acid water has been added ...
has been dryed.
everything else will go smooth as silk.
if you dont get 93% back it will be due to the some of the bromoephed turning
back to phudo when you base the brompephed out.everything else has been done
lots of times
the formation of brompephed from phudo is a 100% everytime.
and is documented in the first ref. to turning ephedrine to meth back in 1927
and grinyards of these type usuly go all the way
hell they are standerd lab. excercizes for 2nd year collage chemistry.
but you must keep the water out untill the end
.that means all solvents that go in that three necked flask get dryed with
sodium sulfate,etc
and your yealds should be way up there.
anyone with experence running grinyards shold be able
to pull this off very easly.
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Rhodium
(Chief Bee)
11-01-02 04:53
No 375356
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Are
you suggesting to form a grignard reagent out ...
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Are you suggesting to form a grignard reagent out of a molecule having an
acidic N-H bond? It will auto-quench itself.
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BenWiFFen
(Line Monitor)
11-01-02 05:21
No 375359
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Hell
the time
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Hell the time it took me to read that I could of made a few grams the old
way.
STUMBLE-BEE
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bbman
(Newbee)
11-01-02 08:22
No 375397
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So
all we need is
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So all we need is chloroform, carbon tet, phosphorous pentabromide, argon,
magnesium metal, and few other odds and ends? This is easier than
getting Li and Ammonia?????
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