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.
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.