How many volumes of acetone would you guys say is required to drop the meoh solubility low enough to not lose product after crystalization?

Who cares, evap your solvent and recover

ˆ it was over a decade ago . . . its was more euphoric than MDA, stronger as well. I went down to the yacht club, with the intention to clean my boat, but just ended up sitting on the stern of my boat watching the other boats come in and out of the harbour for hours. The sunshine seemed almost tactile. Everything was bliss and beauty. Psychedelic insofar as it allowed one to focus on the beauty of details one might not otherwise be aware of, but no hallucinations or mind fuck. I forget doses, but a cap full of this stuff was enough to make conversation difficult. At a party a chick I was talking too asked me "Are you really fucked up on drugs right now?" I was forgetting what I was talking about halfway through a sentence. I know what I'm describing doesn't sound like fun, but it was without question my favourite of all the other amphetamines I've tried (MDA, MMDA, DMMDA, DMMDA2, TMA2).

Well worth the effort to experience.

Oh, don't be so quik to write it off jon. As I mentioned it is much stronger than MDA, which makes the effects almost a magnitude greater than MDMA. It may be my description doesn't do it justice, but comparing DMMDA to MDMA is an apples and oranges comparison.

another question antibody how did you like mmda?
i hear it's like the second part of mda with the relaxation and the tactile enhancement and, very enjoyable.
it sounds like parsely oil is a win-win situation
mmda and 2,5 dmmda
i'll bet the two mixed up would  be a really cool cocktail.

Just a small update...I've tried washing the oxime with 1M HCl like Akcom recommended. I think the oxime was almost dry after 2-3 hours, instead of days. No more fucking around with the oxime not crystallizing for days  

Its off topic and I will split this later if the conversation extends past this post but if you are taking ANY drug and do not trust the people you are chilling with 100% then you need to A: get new friends and B: just dont take drugs with those you dont trust.

Not following either of these rules will imbed a deep psychosis that may never go away. Drugs are tools...

You would not use a hammer and a nail to fix a flat tire and on the same note you should not use a drug if its not the right tool for the time. As soon as drugs are no longer a tool or a treat and become a way of life you may as well quit taking them because you have just wasted the greatest gift nature has given man.

Did you distill your ketone?

The oxime crystals should be snow white . . . if the post rxn product is any other color then there are substantial impurities, which might be why it has taken so long to xtalize. Even when Ab2 had an oil product it was milky white, except when the ketone was not pure.

sexy xtals though

Hey!

@ab I did distill the ketone, but I don't have a fractionating/vigreux column, and to be honest I wasn't very satisfied with the way that the distillation went. There were no problems, but what I collected came over a range of temperature. I did break it up into three 'fractions' when I collected; each flask was a bit different. Nothing major, for instance I still have the initial fraction and the last fraction; they appear the same, but each has a characteristic smell, a bit different. Also have no way of measuring pressure at the moment. No oily white product in this case; it's an amber ale golden.

@NPH I've not done this before. The hydroxylamine was given to me and most of it went into this experiment. If what's crystallizing is the oxime then I will be happy; the crystals look like what you'd expect from a solution slowly evaporating off, they look nice and clean and well formed.

The residual does smell of original ketone or aldehyde.

I'm well out of my depth here. I don't know why things have gone the way that they did, and very much a novice when it comes to chemistry. But I'm glad that I hung to that stuff. I won't want to chuck anything now ... ;-)

if you are unsure which fraction of distilled ketone to use, you can do a sodium metabisulfite test.

thanks for those details ab. I did this test on a small amount of my material. Not with these specific details though, ie. I just used water to make the saturated solution, also I didn't refrigerate. Plus, I really cheaped out on how much ketone that I used for the test; really wasn't happy about seeing that go by the wayside. The tests that I did gave a half ass result. I read in hive posts about a 'chicken soup' kind of outcome.  It did look a bit like that; kind of a slurry. The test tubes sat around (long time) after that and eventually resolved into two layers of liquid. I have done this test in the past with much clearer and more encouraging results.

I'm going to give that another shot with a more generous helping of 'ketone'. At this point I'm not feeling so stingy about it.

And hey, thanks for the input and your original hive efforts and write-ups. I had a hive account back in the day. Hardly posted. I can remember going down the street to post from a community center to avoid having my home ip number associated with any posts that I made. Time flies, that's what they say. ;-)

Opening half year old thread,I hope not in vain...

I found out harder way that oxime precipitation and appearance is HIGHLY dependant on MeOH/H2O ratio and cooling/heating.

First time I evaporated most of the MeOH,added water and stirred for hours at r.t.
I got oil on bottom that became semi solid on cooling and  non-newtonian liquid when thawed.

Tried to reduce that following RoidRage/Chromic writeup and reaction died as soon as I added AcOH(after oxime and everything). WTF!? 
Then I tried to save oxime by filtration/distillation but ended up with some kind of white-tan mud 2x heavier than oxime that is probably part oxime and some insoluble salts.I still don't know what this is but I will try to separate oxime using hot MeOH and filtration later.

Now I made oxime again using Sonsons method but I felt like NaOAc was insufficient(reaction mix was slightly acid,cca. pH 5) so I added liberal amounts of Na2CO3x10H2O until I saw hydroxylamine freebase forming no more,effervescence starting to die off and pH raising at cca. 8.
Played with MeOH/H2O ratio and crystal seeding until oil became large clumps of solid and small crystals floating around.

Will tell you more after I try to isolate it again.
Letting it in freezer for a day or two,followed by filtration (and saving mother liquid in freezer for few weeks,
that is how I got seed crystals in the first place) and washing in water might do the trick.
If I menage to get feather-like crystals that are of the current size drying won't be a problem.
It might become nasty putty if it starts thawing at r.t.