Gassed xylene with Hcl gas till turned red.can be fixed?

pekebaz3 · Tue Jul 12, 2005 11:07 am

Swim gassed mdma.fb/xylene with hcl/h2so4 and the fb turned red Shocked

and acidic.can anything be done to save his batch.I'm sure someone else is having this problem.

bio · Working Bee

No crystals at all? If so it's a dirty batch, everything is wet or both!

You can extract with water then make alkaline, extract again then redistill. Or maybe you didn't distill in the first place?

pekebaz3 · Tue Jul 12, 2005 5:46 pm

no..he did filter a couple times b4 this and got very low yields. he's using h2so4/hcl acid to gas, so no distilation so far this step.he's thinking either there is no freebase left or he ruined it somehow(overgassing, suckback, low ph) just can't figure out what is going wrong.he would be very thankfull if someone could shed some light on this subject.sorry if I was vauge in my earlier post.thanks

DjTime · Chemical Dj

SWIM has had this happen a couple of times. I just threw it out and started over from scratch. It happened twice in a row. So I changed my procedure. I found it was due to moisture in the xylene.

pekebaz3 · Tue Jul 12, 2005 6:41 pm

maybe from weak h2so4?if so should he distill it or try to get stronger acid?

Harmonia · Tue Jul 12, 2005 7:44 pm

Did you dry your xylene before gassing (ie with MgSO4 or any other drying agent)? This is VERY important and must be done.

hAzzBEEn · Tue Jul 12, 2005 8:30 pm

Two threads, one question?: pH while gassing (8:02am/9:21am), Gassed xylene with Hcl gas till turned red.can be fixed? (11:07am).
I'm not bitching, I just feel stupid because I replied to the other one.

anime · Tue Jul 12, 2005 8:56 pm

bio · Working Bee

...........iMO reduce till you have enough to distill. ...........

Hydrochlorides will not distill, at any reasonable temperature anyway.
The oily red mess is the amine HCl if the pH is very low.

Don't throw it out fix it as indicated above. You can reduce first and then base before distillling but the temp of boiling xylene is high which could cause some decomposition, but I'm not that familiar with your product. Easier and most efficient to extract 2-3X with water, wash the water 2X with fresh xylene, if thats all you have, before basing then fractionate slowly with a short column.

primathon · modified

One question, one topic. I took the liberty of removing your duplicate entry.

pekebaz3 · Wed Jul 13, 2005 4:49 am

swik thanks you very much for all your help.sorry for the cross/double post.

MiNdBaBY · Fri Aug 12, 2005 8:36 am

MiNd is gonna throw his advice in here..

MiNd most often working with PEA's, often utilizes an interesting gassing technique. lol

MiNd will gas the NP containing the FB PEA which obviously precip's out during gassing; however, MiNd will 'overgas' to a point where the solute will turn pinkish/red within a couple seconds. This is a sign of excess acid and though is washable from your precipitated compound, MiNd will add (utilizing an eye dropper) the same NP w/fb drop by drop with a stirring until the excess acid is used up via rxn with the new fb being added. This whole process takes a matter of seconds.

In further detail and explanation, prior to gassing, MiNd seperates and stores a small qty of the np/fb mixture in a test tube or small erlenmeyer (25ml) for this sole purpose. MiNd finds this MUCH easier than going to the trouble of having to clean off excess acid from final PEA product after gassing.

This obviously doesn't touch the topic of having a wet NP, thus MiNd will offer an on the spot solution to this situation. Such will require to have some predried (oven baked @ 400 for an hour or so) MgSO4.

IF you have gassed your NP, especially to the point of a redish color, WITHOUT any precipitation, add a small CHUNK of MgSO4 to the vessel. Wait and watch, IF you notice bubbles (very slowly) evolving from the MgSO4 it is from the rxn with & removal of H2O (a good sign). With time the MgSO4 will dry the solution. Then filter as normal the precipitate from the NP. The twist now is that with your precipitate (desired product) in the filter along with the remaining MgSO4, pour thru a solvent that your product is soluable in (alcohol being MiNds choice for his PEA HCl's) with the funnel & filter being over a clean and empty Erlenmeyer or equivalent flask/vessel. Then simply evap that solution in an glass pyrex baking disk for example, or on a plate, dish, etc.

This entire process is easier than it sounds and affords immediate on the spot solutions to both over gassing and/or wet solvents.

Your welcome, MiNd.