Author Topic: Jon's route (Read 3445 times)

igotthere · « **Reply #60 on:** July 31, 2012, 07:34:59 PM »

right so I took the ipa/methylamine soup, it was already at 11.2 ph so I added some dcm. there was no phase seperation so I then thought that If i add some water the ipa will mix with that and hopefully the dcm will seperate out, which it did.
I took the dcm, evaporated that off (lots of smelly methylamine came off).
The temp was at around 40deg c initially, then it slowly went up to around 60, then up to around 80 deg c.

I started getting that familiar mdma smell, there was some slightly smokey smelly mdma vapour coming off.

spices route to the hcl salt is as follows:

evap dcm off to leave mdma freebase which is sort of 'olive oil' in consistency.
add equal parts 'dry' ipa and titrate to ph 6 using hcl dropwise.
evap ipa to get a gummy mass. be careful not to scorch product.
add roughly 10x super dry acetone and move everything around, then bingo - mdma hcl.

So I added equal amount of dry ipa, then added hcl dropwise.
disaster - with only two drops it went from 7.2 to 1.2...
i don't know how this will affect the formation of the mdma hcl but after evaporating off the ipa I wasn't left with a gummy mass, it was very much the consistency of olive oil still.
On tasting it I had that familiar horrible taste. spice says it should burn my tounge and it does.
I'm very wary of adding my super dry acetone though, in case I need to do something to it before this stage.

igt

igotthere · « **Reply #61 on:** August 01, 2012, 06:23:00 PM »

I added my dry acetone and got nothing.

A couple of questions:

It wasn't ice cold acetone.

my titration went horribly wrong and the ph plummeted from 7 down to 1.2. How would such a low ph affect crystallization?

I have another piss yellow jar that I hope to work up tonight.

Do I flood this jar with water BEFORE setting my ph to 12? or do I just ph to 12 before extracting with DCM?

igotthere · « **Reply #62 on:** August 01, 2012, 06:28:48 PM »

sorry t cowboy just re read your post, so am going to evap the ipa off first then add equal parts water then ph, the extract.

Electro´S · « **Reply #63 on:** August 01, 2012, 06:48:40 PM »

why don't try with dry HCl gas trough the solvent?

(H2SO4 - ClCa)

igotthere · « **Reply #64 on:** August 01, 2012, 09:27:38 PM »

Electro

I'm a little nervous about gassing, quite a few people are saying that its quite finiky..

Electro´S · « **Reply #65 on:** August 01, 2012, 10:33:45 PM »

Quote from: igotthere on August 01, 2012, 09:27:38 PM

I'm a little nervous about gassing, quite a few people are saying that its quite finiky..

It is the same than methylamine/IPA. and you can not over acidify if your gas is dry.
I know than when you are trying to gas something like pyridine (very very hygroscopyc) is a pain in the ass, but for MDA or MDMA i think it is the way of the winers.

T-cowboy · « **Reply #66 on:** August 03, 2012, 03:34:58 PM »

HI friend as i can see you have some trouble pertaining this route, i think it will be easier to pm each other.

Was that familiar mdma smell, like licorice? i ask this because iodosafrole/bromosafrole tend to reform (polymerize like volcano "stuff") (hence the smokey thing you saw maybe?) on adding heat, returning iodosafrole/bromosafrole to its original state : Safrole/isosafrole : smell : licorice like. Hence the mdma smell maybe. I am just speculating, but it sounds about right

So i take it you got nothing from the first batch, because of work-up. this should be no problem, if there is any mdXX in the solutiun somewhere, but since you used dcm, like the way you did i really cant help you on that one / sorry bro :/

how are this with the second batch? i just re-read Jons original statings about the work up and passed them on to you.

igotthere · « **Reply #67 on:** August 13, 2012, 09:39:38 PM »

Hi All, sorry for dealy in an update, very very tricky to get online safely sometimes, now all packed away and waiting for another window in which to experiment.

So briefly, I failed.. I think the prob is lying with my finkelstien to ido, as I've never really seen a nice purple idosaf?
Someone has pm'd me suggesting that the issue may lie with my use of kI rather than Nal. does anyone have a view on this?

igt

igotthere · « **Reply #68 on:** August 13, 2012, 09:48:54 PM »

t cowboy, thx will pm when back up and running.
I was getting licorice type smell, although temps never went past around 80 deg c which I think is ok? this smell/vapour was coming after I was evaporating solvents. Smelt very similar to the smells that were apparent when working up from benzo wack-al/hg route.

igt

p.s. didnt get your pm regarding jons notes

mdhard · « **Reply #69 on:** August 14, 2012, 12:36:39 AM »

I had the same problem to crystallize mda ...

add the same amount of IPA dried to freebase, then evaporate the IPA (pH 6)

but no crystals appeared ... I lost 100g freebase test ...

Next time I'll try hcl gas

spice · « **Reply #70 on:** August 14, 2012, 11:30:03 AM »

I read you posted this at another site. You didn't lose product. You said you got a gum or paste. THAT WAS YOUR PRODUCT.

Using the titration method works better for mdma but mda crystallizes this way too....but you have to use dry acetone + stirring to remove the water residue that is makijng it a paste.

mda crytsals are finer so it is not as easy as mdma.

I have written this method up exhaustively all over the internet.

If you gas and there's water ANYWHERE you will have problems there as well.

Sneak · « **Reply #71 on:** August 14, 2012, 12:53:30 PM »

Exactly. I thought that's what you said. Acetone wash the gum to see the crystals burst into existence.

Lick the spoon. Boom.

Wizard X · « **Reply #72 on:** August 14, 2012, 01:37:19 PM »

mdhard · « **Reply #73 on:** August 14, 2012, 05:43:15 PM »

Quote from: spice on August 14, 2012, 11:30:03 AM

I read you posted this at another site. You didn't lose product. You said you got a gum or paste. THAT WAS YOUR PRODUCT.

Using the titration method works better for mdma but mda crystallizes this way too....but you have to use dry acetone + stirring to remove the water residue that is makijng it a paste.

mda crytsals are finer so it is not as easy as mdma.

I have written this method up exhaustively all over the internet.

If you gas and there's water ANYWHERE you will have problems there as well.

hi great "spice" it's okay with you?
I read all your posts on another forum, you really are very good

I believe now after reading so much that the big problem was that it contained water ..

I lost all my freebase, because I threw away the goo then = [
Now I know where I went wrong I will not make the same mistake again ..

Now I understand that it really needs to be 100% dry ...

thank you very much

Sneak · « **Reply #74 on:** August 14, 2012, 07:19:07 PM »

Omg I did not just read that!!! My heart just sunk.

Oh shit. Some rats had a major party down the drain that night.

mdhard · « **Reply #75 on:** August 15, 2012, 12:01:59 AM »

Quote from: xxxyyy on August 14, 2012, 09:30:25 PM

Quote from: mdhard on August 14, 2012, 05:43:15 PM
Quote from: spice on August 14, 2012, 11:30:03 AM
I read you posted this at another site. You didn't lose product. You said you got a gum or paste. THAT WAS YOUR PRODUCT.

Using the titration method works better for mdma but mda crystallizes this way too....but you have to use dry acetone + stirring to remove the water residue that is makijng it a paste.

mda crytsals are finer so it is not as easy as mdma.

I have written this method up exhaustively all over the internet.

If you gas and there's water ANYWHERE you will have problems there as well.

hi great "spice" it's okay with you?
I read all your posts on another forum, you really are very good

I believe now after reading so much that the big problem was that it contained water ..

I lost all my freebase, because I threw away the goo then = [
Now I know where I went wrong I will not make the same mistake again ..

Now I understand that it really needs to be 100% dry ...

thank you very much
MD one thing I learned from my first run at this stuff is forgive the E shout but it's needed here NEVER EVER THROW OUT ANYTHING UNTIL YOU VERIFY WHAT IT IS THAT YOU ARE THROWING OUT. If you had a paste like substance all you had to do at that point I would think is either hit underneath a pyrex pan with a blow dryer while your paste is inside also cover the pan with aluminum foil. or Allow it to thicken up naturally by leaving it sit for a couple days and then it would of theoretically naturally dried. I am sorry for your loss man my condolences go out to you and your wallet. Hey at least you didn't get crystals that tasted like fish salt ... thats what happened to me I got all the way to the end and eff'd up on my wacker oxidation A/B extraction and got me a nice beautiful mdxx inactive salt. Also try using a smaller batch next time and do a test batch with 25 or 30 Ml of base and then use titration to obtain desired PH... I only used dried IPA/HCL and my inactive product still salted out with a little heating some time in the freezer and then natural drying for 18 hours. You can always correct your PH level by adding more base to the solution I think.

hello okay with you?

I threw everything away because I got frustrated, hehe ... but I know it was active! =]
I experienced a bit of goo and it was great!

I did exactly as you said ...
but the secret to "spice" it said in acetone then added to goo ..

I left the goo covered for 24 hours and nothing happened ..
Next time everything will be OK with anhydrous acetone

I'll write in the forum when it succeeds

thank you to everyone who helped me ..

Shake · « **Reply #76 on:** August 21, 2012, 04:21:14 PM »

i have thrown heaps of goods away not nowing it contained a shitload of product... the water extraction is the only fool proof method.. i think forget the rest!

jon · « **Reply #77 on:** August 23, 2012, 03:06:50 AM »

i see you guys hitting the mark but missing it on workup you need to evap all that methylamine and alcohol using an aspirator then it's just a simple acid base extraction a water wash and it's pure enough right there to use.
and yeah i like the freebase.
and with finklestein reactions the trick is copious acetone lots of it and good stirring.

jon · « **Reply #78 on:** August 24, 2012, 07:42:51 AM »

i used shittons of water to workup the ipa mdma soup this works well but stinks like hell.
just use my previous suggestion.

Electro´S · « **Reply #79 on:** August 24, 2012, 07:13:32 PM »

Hi Jon.
What is the exact molar ratio MeAm- Iodo safrole - IPA

I think 15/1 MeAm/Iodo Compound is in somewhere, but the amount of solvent is unknowed for me.
Is this one the rate???

Author Topic: Jon's route (Read 3445 times)

igotthere

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Electro´S

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