MM failure.

[FlaskGenie]

Swim has a failed MM dream.  Benzo went fine.  Bisulfite test positive.  Al/hg went as planned as well.  Xylene used as non polar.  MM to the Ts.  Swim  thinks here is swims problem.   Swim has been advised  that A/B and distillation should be performed before gassing.  So swim takes small amt of 35% Naoh and adds to non-polar and cks w/ ph paper.  Ph = 14 (black).  Swim then takes. Dh20 and adds dropwise 31% Hcl untill ph is ~5.  Swim then washes non-polar X2 100ml. w/ acetic water.  Then adds 35% Naoh to water washes untill ph is 14.  Swim then performs X 3 50ml extractions w/ DCM.
Swim thinks this is standard A/B but w/o any chem background swim has doubts.

DCM is stripped off at atm. Then later weak vac was added to get the last of dcm out.  Next day swim sets up dist. w/ asp. vac and more DCM comes over.  Swim brings heat up slow w/ water bath but steps away for a moment.  Swim comes back and temp is at 58 and there is a water clear liquid in receiving flask.  Smells and looks like dcm but what does swim know. There is not much of it 6 gms or so, it is not washed w/ water to test (should have).  Thinking these are the goods swim dump the stuff into acetone to gas and nothing happens.  Swims question is where did he go wrong?  Xylene and all washes were saved.

[OcoteaCymbarum]

When you have the base in the np here's what you do.

First, wash the non-polar with 5% NaOH a couple of times. That way, most water soluble impurities are washed away.
Then you extract the np layer with 10-15% HCl, about 5-10 times in weight of expected freebase.
That way you form the MDMA*hcl salt, and it goes in the water layer.
Then you wash the water layer with a little np fresh from the bottle. To make sure no np impurities were carried over.

Then you take your water layer and with strong NaOH(35% for example) you slowly bring the pH to 12-13. You will see the oil fall out, sometimes if very strong NaOH is used, or if you overbasify, the oil will start floating. Its brown and cant be missed.
You extract again with non-polar, then dry and gass.

So the making of the hcl salt is required to extract from the non-polar.

[FlaskGenie]

Followed your advice OC and after adding 35%Naoh some brown Particulate matter fell out.  Is this the goods or did i just make NaCl and water?

[OcoteaCymbarum]

thats freebase. Its brown right now but if you distill it, it will be crystal clear.
When you basify the water layer containing the goods, it turns milky white with a brown oil falling out. When you back extract that water layer, it will turn almost transparent so you know your base has been extracted.
NaCl is white, never brown

[FlaskGenie]

Here is what happened.  There are small oil droplets liberated by the naoh and this layer of stuff also fell out.  The stuff won't go into the dcm and it won't go back into water so I guess it is trash.  The dcm is dark brown so I will strip and distill and report back.

[FlaskGenie]

I am trying to distill the mdma but am having trouble finding safe perams to distil.  Any ideas?  BS says never go over 120 w/ vac.  but another source says it comes over at 158 w/ vac.  Im flyin by the seat of my pants. ~O~

[FlaskGenie]

OcoteaCymbarum,
You were right. Swims not so effective a/b left the product in the non-polar (Swim is glad he saved it).   He Used your a/b advice and what do you know, ther was swims goods.

Thanks