SWIM is tired of failling, he needs help

[kewlcanuk]

(Push/Pull Meth syth)
Swim's I2 doesn't react with the RP. No smoke nor any visable reaction of any kind. Also I2 doesn't fully desolve in the DH2O mix.


Can someone help swim?


THX in advance

Canuk

[p2e3r4f5e6c7t8]

Did swim have nice clean reagents to begin with ?

And now all of swims chem's are already mixed in his reaction flask, Maybee he should just do a refluxx for 48 hours then work it up and see if swim has toalty wasted some chems and feedstock.

Swip thinks that the reagents used were not clean enough(pill gacks or something)

[kewlcanuk]

The pills were definatly extracted properly...water and methanol distalation. But...I did not wash my RP. Could that have been the problem. Also... my crystals were clumped together and slightly moist, is this normal?

[Scottydog]

Swim's response is theoretical, it is obvious that your discussion is not!  

Nice gas can, push/pull unit. Those barbed PVC tubing connectors and hose clamps look familiar. The glass jar you are using doesn't look entirely safe. Someone viewing this "might" want to replace something like that with a $12 flask and rubber stopper?

If you say your E is clean, then what about the water ratio? How much water was used in the rxn? What were the ratio of chems? RP from what source? (Matchbooks, labgrade) How many times has the RP been used before? Is this an oil or water bath and what reflux temps were reached during the course of the rxn?

Swim has dreamed that excess water and pill gakk will kill a reaction dead in its tracks.

Pretty picture but not enough info...

Canuk, so you are Canadian? I have heard that as long as there is no finished product that a rxn as pictured above is not illegal. Is this true?

[kewlcanuk]

Water bath... Ratios: 2p I2(2g), 2p P(2g), 1p RP(1g), 60ml dH2O. RP is fresh and from MB. As for the jar... it is the best swim can do. City of 30,000 no cooks, no science stores, nothing. Swim did not reach any temps but was shooting for a low 150 to 180. Swim never made it that far as there was no reaction off the bat... which it was swims understanding that there should have been.


Thanks,

Canuk

[biotechdude]

HEAT IT UP!!

If your precursers are damp it wont magically start reacting at room temperature.

Slowly heat it up and see what happens...

[12cheman12]

WOOOWWWWWWWWWWW MATEE did you say 60ml DH20?
and your doing a 2 gram reaction?
And you tried to do a Push/Pull

60 mls is way to much, try something along the lines of 1.5mls and reflux for 24 hours.

[Ewok_Poacher]

I would definatley say that you flooded it, swim measures by the drop of dh20.

[evilscripter69]

if the I is from tincture dont add any water at first
get it reacting and when it looks dry, and or u see white crystals add water about 1cc at a time with syringe in hose
observe reaction inbetween each addition.with what u have now a reflux is best option
And yes heating it will work too, try using a sand bath to heat it, you can envelope the flask partially, and also monitor temperatures

[evilscripter69]

SWIM will post a ghetto microwave/fume hood, All fumes pumped into sewer system. You could kick off reaction in it without making noxious odors, the rig is capable of boiling 2 liters of xylene to 110 degrees centigrade without a hint of smell, only smell comes from opening door

[kewlcanuk]

Swim is going to try again as swim has some reactints left. He'll post and let you know how it goes.

Thanks again for all the replys I'm glad I tried this board.


,Canuk

[p2e3r4f5e6c7t8]

Now that swim has seen your ratios he was wondering why such a large reaction vessel when only a NANO reaction is being preformed ?

Or has swip missed something ?

[kewlcanuk]

Swim will down size. He designed this apparatus to do way larger amounts. He just wanted to make sure that he could do it before he invested to much money.

Swim is very new to this, never ventured outside anything that didn't come from a plant or that couldn't be blown up in his back yard.  

[barkingburro]

dont use the d/h2o, use a few drops of h2o2, ok a few ml. there is d/h2o mixed with the h2o2 and the h2o2 will help kick thingts off for stubborn reactions.