iso behaving like it should but is it really...

[dave1234]

[ApprenticeCook]

apart from solvent you told us nothing about the storage of the material.
I love these 'shot in the dark' question/answer problems.

Temperature, light exposure, container type and material, sealed?, acetone quality (store or lab grade?), storage enviroment.

So the iso distills at the correct temp (vacuum used in disto?) and you made it to mdp2p (how? what method? how did that go? correctly as per synth document indications?)
what colour was it? (this is interest based, as i said recently, the colour of mdp2p is varied and not reliable indicator in most cases).
Did you test with bisulfite? what result?
What grade reagents did you use to produce it?
What conditions were the reactions run at?
What equiptment did you use?
What was the shape of the cloud above your house at the time? (joke)

What process did you do to run mdp2p-->mdma freebase ?
(same questions for this as for mdp2p reaction question)

Jesus include details and set it out clearly, your post was bad and to hard to read, otherwise no one will care enough to read your post, little alone help.

-AC

[dave1234]

maybe I need to simplify my primary question :
Is isosafrole stable sitting in a  sealed PP container with acetone, for a few months?

[Rhodium]

Is isosafrole stable sitting in a  sealed PP container with acetone, for a few months?

It should be rather stable in acetone, at least as long as it was pure (no acids present, etc.) and that the solution was stored out of direct sunlight, not too hot (the usual precautions).

[dave1234]

[dave1234]

Is there any problems with re-refluxing my isosafrole over vacuum with KOH...in case it all has'nt can verted to iso?
What is the best way of extracting the KOH from the isosafrole...can it be filtered (because I realise it is broken down) or a vac-distilled which needs to be done anyhow  will be best and a little less time consuming??

[dave1234]

So the iso distills at the correct temp (vacuum used in disto?)
Unfortunately back then (it was a large batch) and wasn’t under vacuum…it’s boiled at what I think was the correct temp but later did I found out that the thermometer was inaccurate.  Gave me loads of grief…which is nice.  I refluxed the Safrole with Butanol and KOH (solution from a hydroponics shop…I uneducated decision).  It turned dark after a few hours and I thought and still think the reaction was complete.  Distilled it back it approximate 100% yield of clear isosafrole. 


(Same questions for this as for mdp2p reaction question)
Performic oxidation

Did you test with bisulfite? What result?
It was successful but only once I used some small amount of alcohol.  Crystallized into yellow sludgy small crystals or maybe what is ‘chicken fat’.

What process did you do to run mdp2p-->mdma freebase?
Al/Hg with Nitro etc.


What grade reagents did you use to produce it?
Lab grade
What conditions were the reactions run at?
Under vacuum from after the reaction to isosafrole.



Thanks rhodium. That my iso should be fine helps me sleep a lot better at night.

I think with all the tests I have run, everything to the end process seems prefect…colours, bp’s, conditions etc.  

Going straight from my final washing’s of my AlHg reduction and following Methyl Man’s notes directly to crystallizing…I think my problem lies with trying to crystallize 20g of MDMA in 700-1000ml of solvent. 
With no more MD-P2P left it’s back to the drawing board…
I love it how a fail on the final and most simplistic part….