Milky post reaction fluid

[asuena]

What a horrible nightmare i just had. In my dream i decided on a 10g LWR with ratio 1.3 : 0.5 : 1.0 : 1.0 (I : RP: E :H20) all Lab Grade including the ephedrine (or so I was told). I had similar dreams in the past with great results even when using gaked psuedo.

After refluxing for aprox 28 hrs at about 100 - 105 oC with everything looking and smelling the way it should a strange thing happened. When i diluted the post reation fluid with warm ater if turned milky white. A white crystaline prcipitate fell out of solution big time, most of the RP fell to the bottom of the flask as it should but some remained in what seemed to be an oily film on the surface.

It took about 100 ml of boiling H20 to dissolve the precipitate so it would go through the filter but as soon as it did and cooled it came out of solution again. What the fuck is it? I decided to base it and when the pH reched 7 there was no more precipitate after  which I added toluene and worked up as usual and got nothing. Even the mystery crap didn't come back.

The ephedrine looked and tasted like it should but after what just happened I can't help but conclude that was not ephedrine. Period!
But perhaps I fucked up somehow...

Did anyone of you more experienced Bee's ever witness such a thing?  What are your thoughts? Am I correct in my assumption?

[12cheman12]

you said the PH reached 7 and you worked up as usual, do you mean you pulled your NP while the ph of the rxn fluid was 7, because you know your goodies dont move over till a PH of about 12 or 13.

[asuena]

Yes. I based it to a pH of 13.

[12cheman12]

swim has seen problems like that, normaly when the pseudo isnt clean from the start.
maybe you should of recrystilized your pseudo before you put it in so youd know for sure what you were playing with.
You said you tasted it, and it tasted like pseudo, but maybe someone dodgy cut it badly so there was hardly any pseudo but the taste would still come through.

[asuena]

thanx for your imput but it wasn't psuedo it was ephedrine from a trusted source...come to think of it it was my first synth using ephedrine instead of psuedo.

Perhaps the ratios for a LWR would change when using ephedrine or perhaps I fucked up. I have to be certain before I go and tell someone they gave me garbage.

I forgot to mention in my first post the RP and iodine reacted violently in the begining of the reaction (its been a while and i just dumped the whole amount of iodine in all at ounce) perhaps my ephedrine burnt up.

PLEASE COMENT

[ChemoSabe]

Essentially it was not ephedrine.

Otherwise you would have gotten product even if it was tainted.

Ephedrine is not so far from pseudo that you would have gotten such different results.

You got screwed at the point of sale.

The suggestion to have recrystallized it before the reaction was a decent one.

Actually I just realized that I missed your comment about the violent reaction at the start. Did it produce a lot of weird looking smoke? Usually it's only a true flask fire that will destroy the precursor. If you get the classic "bleeding flask" symtoms the reaction will usually go OK if you reflux it for long enough. If you truly had a flask fire that could bee the problem though. Not sure.

Searching on flask fire might get your answer. Flask fires are quite rare though and rather intense. Not to bee confused with "phase 2" of a hot, dry cook.

PS. I'm not certain of this because I never had one but I think that if you truly get a flask fire that not only will your precursor be toast but so will all of your reagents. Someone else will have to confirm that though.

[asuena]

Thanx chemosabe,

There actually was some weird colored smoke as a result all of the iodine reacting at once. At one point i thought the ballon atop the condenser was going to burst due to the amount of smoke generated. There wasn't much i could do as i wanted to avoid all unpleasant odors at all costs.

But you're right i sould have gotten something back and didn't. But there's still one question that i would really appreciate someone answering.

Could it be possible to screw it up to the point where adding hot water to a warm post reaction fluid would cause a shitload of precipitate to fall out of solution. I'm no chemist but it just doesn't add up. How could whatever that precipitate was fall out of the post reaction fluid by diluting it with more water. I don't get it.

[12cheman12]

if you had clean ephedrine, RP and I2 then adding hot water to the post reaction mixture would not make anything precipitate out. Even dirty RP and I2 still shouldnt make anything precipitate out.
The only real thinkg swim can think of is that you ephedrine was dodgy, its the only explanation.

[ChemoSabe]

My understanding of a flask fire is that your RP actually ignites when one occurs. Tons of smoke is produced. Usually enough to burst your baloon and to alert the fire dpt.

If you had any usable RP leftover it wasn't a flask fire so you got screwed.

Unless I'm incorrect on the nature of a flask fire this should end all speculation

[rangahtank]

SWIR has had the milky result as you have stated.  Leaving it set, ph 13 with naptha above the filtered reaction fluid for several days has eventually yielded some surprises.  Try it.

[wareami]

with an exception or two or 4...
ChemoSabee is correct on a few observations...
A full blown flask fire is rare...to the poin6t of ingnition that is.
The term flask fire more or less indicates that a fire could be eminent. It's a term used loosely for lack of a better term. RP it would seem is the Heat producing agent in this scenario....so it's easy to blame FIRE on the loss of goodies when the rxn wasn't properly ratio`d, hydration-wise, from the GitGO.
Ibee's toasted one rxn early on when he was just a wee little pyromaniac bee playing with excess LGRP.
Because of all he read to that point, he knew what to do in order to keep things from getting out of hand.
At the point the flask filled completely with verydark RED almost purplish smoke, he knew what was happening and immediately quenched the rxn with dh2o.
Yields suffered greatly when weighed against the expected.
The excess h2o was poured off, the rxn allowed to progress as normal and RP was recovered following the final work-up.
The degree of precursor loss is determined by how long the rxn is allowed to proceed under those violent conditions due to off-balanced ratio.
Small toast rxns will eat a percentage of the precursors and feedstock.
It's unlikely that the RP will be used up under prefire conditions but it's highly likely that the feedstock will be consumed until an equilibrium is reached at which point thngs begin to subside.
There are no definate numbers as each rxn is different depending upon hydration conditions to start with.
Needless to say....Ibee's experience occured during a Hot/Dry fast HI/RP.
Some early rxns such as this are thought to have contributed to low yields because Ibee alays thought a violent take-off was a good sign.
Then he read the differences reported by the elderbees when discussing fast/violent versus slow and controlled rxns.
The slow controlled reports always had a higher yield common denominator.....and so beegan the Hunt for the LWR as we know it today.
This solidified the importance of weighing everything out properly and starting with tried and true ratio's based on the rxn at hand!
Bees will also read reports from those more experienced with the Hot/Fast P/P, that making HI first(aka pre-firing) is favorable because any likely violence that might damage the E is lessened if the E isn't present at the time the critical exothermic part of rxn occurs.
Makes sense to Ibee

[ChemoSabe]

Swim was doing a reaction of his last semblance of recycled LGRP and the thing nearly immediately violently erupted upon getting hit with a little atomized spray of water. Luckily it was a small (maybe 5g) reaction but produced quite a bit of smoke and stink nontheless. 

Refluxed it for maybe 4 hours after shaking down and mildly flooding. This was well before the daze of LWR popularity so that was swims original experiment with flooding and fluxing. 

Swim ended up getting OK yeild from it but the rp turned into a weird gunky grey/purple plasticy clay-like garbage that could not be cleaned up or used again. It was some rather used RP but nothing like that had ever happened before and has not happened since.

But swim now never lets the RP get that old and haggard anymore and always it's spanking fresh or at least rejuvenated with a portion of fresh (albeit MBRP now instead LG).

[Gluecifer]

Bees will also read reports from those more experienced with the Hot/Fast P/P, that making HI first(aka pre-firing) is favorable because any likely violence that might damage the E is lessened if the E isn't present at the time the critical exothermic part of rxn occurs

This bee is well experienced in the push/pull and never liked the results making the HI first in the push/pull.   However, that is how he now refluxes, by making HI first.

Swim read old posts regarding adding the E first and I second. He then add the red in increments and at last water(with stirring throughout process).  This is how he says his push/pulls were carried out.