SnB Woes...I'm at an impasse and need help

[Rollin88]

I'm having the exact same result on all of my attempts at a one-pot methamphetamine synthesis following the procedure found HERE.

Everything seems to go well, but when I gas my non-polar, it clouds the solution the instant my tube goes into the flask. The precipitate isn't crystalline at all, rather it's a white waxy substance that after filtering and scraping off the filter paper smells like PSE when burnt (not smoked....). I need to know where this wax is coming from.

To purify and concentrate my PSE, I used the ion-exchange method with high acid, cation replacing water softener beads from DOW chemical. The PSE it produces looks fantastic, white, needle-like crystals, but it tends to stick together a bit to itself (meaning, if I dumped 3g in a funnel, it would kinda stick to itself a bit and might need a little shove with a glass rod to get through the funnel stem). My first thought was the cation-exchange water softener beads method is compromised, and they added an ionic 'gak' to the mix which gets eluted from the beads along with the PSE. Since the waxy substance is white and was evenly distributed amongst the pse crystals, it went un-noticed, and it does something to ruin the reduction reaction. Having said that, when I gas at the end of my PSE purification procedure, I get no visible wax at all. It might be there, but at least i'm gassing out a crystalline amine along with it. After the SnB reaction fails, why isn't the PSE gassing out in the same manner it did during purification? Instead, All I get is wax, no crystals what-so-ever after my SnB attempt. I've tried using hexane/ether, and napatha as my NP, exact same result.

Does anyone have any suggestions on removing this wax from the PSE with everything else removed already? The ion-exchange method eliminates everything but that I think. I ran some tests on the PSE I thought was pure, and it takes way to long to dissolve in IPA so the crystals have to be coated in something.

 

[Nasty19659669]

Rollin88,
I think your problem is the pse itself combined with needing dry HCL gas. The 24hr tabs have povidone in it that will rob your goodies! It must be steam distilled prior to reaction. Also if you are not bubbling HCL from RV through another stop through more SA it will be wet when gas gets there. Poof...no Bueno. Goodies are super h20 sensitive. Try it out. See what happens!

 

[YoSpumoni]

I'm having the exact same result on all of my attempts at a one-pot methamphetamine synthesis following the procedure found HERE.

Everything seems to go well, but when I gas my non-polar, it clouds the solution the instant my tube goes into the flask. The precipitate isn't crystalline at all, rather it's a white waxy substance that after filtering and scraping off the filter paper smells like PSE when burnt (not smoked....). I need to know where this wax is coming from.

To purify and concentrate my PSE, I used the ion-exchange method with high acid, cation replacing water softener beads from DOW chemical. The PSE it produces looks fantastic, white, needle-like crystals, but it tends to stick together a bit to itself (meaning, if I dumped 3g in a funnel, it would kinda stick to itself a bit and might need a little shove with a glass rod to get through the funnel stem). My first thought was the cation-exchange water softener beads method is compromised, and they added an ionic 'gak' to the mix which gets eluted from the beads along with the PSE. Since the waxy substance is white and was evenly distributed amongst the pse crystals, it went un-noticed, and it does something to ruin the reduction reaction. Having said that, when I gas at the end of my PSE purification procedure, I get no visible wax at all. It might be there, but at least i'm gassing out a crystalline amine along with it. After the SnB reaction fails, why isn't the PSE gassing out in the same manner it did during purification? Instead, All I get is wax, no crystals what-so-ever after my SnB attempt. I've tried using hexane/ether, and napatha as my NP, exact same result.

Does anyone have any suggestions on removing this wax from the PSE with everything else removed already? The ion-exchange method eliminates everything but that I think. I ran some tests on the PSE I thought was pure, and it takes way to long to dissolve in IPA so the crystals have to be coated in something.

Rollin88 When requesting help to determine a solution to gakk from pills in a reaction product, we must know the brand name, dosage, and duration of action listed by the pill manufacturer. This is at the very least of required information. Please list all of the inactive ingredients from the package you obtained so that we may better understand what you're working with. Without that information, all anyone can offer you as far as advice will only be based on assumptions and speculation, not actual facts.