Author Topic: removing koh from iso  (Read 2522 times)

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Jasium

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removing koh from iso
« on: October 21, 2001, 09:42:00 AM »
does anyone know of an ez way to remove koh from iso without distilling. heres the dilema. have been thinking of giving Lt's buffered performic a whirl at the 1 gallon scale, and understand from reading here that the conversion rate is high enough to not have to distill the iso, which is very time consuming. i have 98% sassy out of the drum which has never needed distilling for benzo work. i think that the iso would bee ok at a large scale ie. i can live with 60-70% mdp2p yields. i just want to  remove the Koh without distilling. would a brine wash or 4 followed by a few distilled h2o washes remove it? or would it just form a big messy emulsion. i remember back in the day washing sassy with naoh then distilled h20 to remove the eugenol.distilled h2o washes seemed to remove the naoh quite well. please let me know asap bees. btw this is swims first performic, he's been cooking for many moons but never done the performic. sounds good though, hopefully the tone from performic will be more pure. benzo tone dosen't yield as well as the imported stuff in the nabh3cn mda runs.it works well in the nitro ex. 180-185g out of 200 in the nitro vs 200+g's with the labgrade tone. and 600g out of 1000g with benzo tone and 700+ with the good stuff in the nabh3cn. maybe the yields will improve with the performic apple juice.
thanks all
j

"a peeping tom at the keyhole of eternity"

Osmium

  • Guest
Re: removing koh from iso
« Reply #1 on: October 21, 2001, 03:07:00 PM »
I can't recommend taking such shortcuts. You have to distill the ketone anyway, so don't try to tell us you don't have distillation equipment. Distilling the iso-sassy is fast and a real no-brainer when your safrole was pure. It's also the easiest and cleanest separation method.

Jasium

  • Guest
Re: removing koh from iso
« Reply #2 on: October 22, 2001, 06:55:00 AM »
yes os i have a hi vaccum system distillation system with a glas-col. the only reason i was asking was in lt's writeup he said the iso woulden't really need distilling because of the high conversion rate to iso.the only reason i've never done the performic was having to do soo much distillation. but if it is necessary i will do it without hesitation. btw thanks for clearing that up. i guess i should stick with the old adage "if something sounds too good to be true, it probably is". i will get on it and report results.
regards
j

"a peeping tom at the keyhole of eternity"

LaBTop

  • Guest
Re: removing koh from iso
« Reply #3 on: October 25, 2001, 07:29:00 AM »
Jasium, I told you 2 times in PM's to DISTILL the raw Isosafrole, and in the write-up in "the Sequel" you can read very well in BOLD characters that you must always DISTILL your Isosafrole to get rid of any unreacted Safrole and more importantly, any KOH. If there is KOH left in your Isosafrole, then you can forget any good yields in the next steps, conversion to MDP2P and especially the imine forming from your MDP2P.
Washing your Isosafrole/KOH with water or brine(concentrated NaCl/water) will saddle you up with an immens emulsion, which is very difficult to clean up. Only if you really don't have any form of vacuum you should try it, but in fact, if you want to do a performic and the amination it would be very strange to even think about not using vacuum distillation, you need it in several steps.

The use of brine is redundant here, it will not remove any KOH. Only a shitload of slightly acidic water solution(5%) could do the trick to convert the KOH to the salt, which would then solute in the wash water. Strong acids would be dangerous to use, the double bond bridge in your Iso would break up. So no HCl or H2SO4 5% solutions. And with weaker acids you really would need immens amounts of 5% solutions to get all the KOH converted to salt.

So, always use DISTILLATION, under vacuum is ofcourse far better than plain atmospheric distillation. LT/

WISDOMwillWIN

Jasium

  • Guest
Re: removing koh from iso
« Reply #4 on: October 25, 2001, 04:47:00 PM »
thanks for clearing that up Lt, well distill it is! after that that everything is pretty straightforward.will run it and post back results.
j

"a peeping tom at the keyhole of eternity"