I need help with my first MDMA synthesis. PLEASE

togeter

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Hi,
I did my first mdma via nabh4 too,
after distilled mdma freebase at 160c (my vaccum source is quite weak) then i got clear colorless oil at the?
btw i try to gas hcl and got crystal that look very clear (white crytsal)!
after test the result 200mg withour recrytalbut im feel the effect is weak.
So now i dont know what process is mistake. Can someone confirm me that mdma freebase colorless color is correct? or may i broken freebase at 160c disilation?
Is there any chance that i left the methylamine freebase in the mdma freebase, then it react with hcl to form methylamine.hcl that contain in my product? may no methylamiine left after distilation right?
Should i wash the mdma freebase with something again to clean it ?
Please give me some help
 

Pororo

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Mdma fb must be colorless and there is no chance to damage mdma molecule while heated up to 160c.
I don't think you got methylamine in your mdma, I would rather believe in pmk) Any way, methylamine has a specific smell that you will not be confused. It is not anise smell, it is "rotten fish" smell.
Does your mdma hcl change color (turn brown/black while heated - exposed on the heat source more than 1 hour? You may set your mdma hcl + water in proportions 1:1 on the heat source in the flask and keep it for 1 hour to see what is happening. Flask shall be open!
 
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Pororo

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You need to prepare NaOH in water, 20% ww is ok. I.e. it is 20g of NaOH + 80g of water.
You need to know exact weight of this 20% at the beginning. 20g total for example.
Then you dissolve your salt in water and star adding your 20% NaOH in small portions till PH is 11.
Now you can find out how many g of 20% ww solution was consumed and estimate molar weight of your salt.
 

lucas_cash

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Did you use pmk oil or pmk powder from the start? can you type in the steps you took so we can see where it went wrong
 
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togeter

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I used pmk wax! im pretty sure distilled mdp2p is correct, cause i already know the smell of mdp2p

Im follow this step:

I think about a step that may i did wrong
- After finish reaction (finish stir 2h after add nabh4) then i realized that my reactor is not big enough to contain all water to wash ("- Add the water and continue mixing during 5 min") so i just add water with less than the volume of btcboss method a lot ( i was thing the wash water process is not important)
- Then i added dcm to extract but dcm get clear color
- I think i did something wrong, may will throw all to the drain
- Then i do some research, realize that may fb is disolve in methanol, and methanol is miscible in the water ! and may i need add more water to make fb out of methanol to catch it in dcm
- yeah, after add more water, i start to get dcm at bottom with more color like its contain freebase
- after that, i distilled the all extracted and get clear oil at 160c

* May i add dcm before wash with enough water is stupid :cry:
* May something go to dcm before it get wash by water :cry:
 
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lucas_cash

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I think you lost your fb while washing.
If you did the NaBH4 correctly.
Than your fb oil will get heavy because of the NaBH4. So while washing and adding the dcm you will see that your oil will separate from the water.
The oil will drop to the bottom and the leftover dirty water will stay above. This way you know that you made the fb correctly.

After separation you can heat up the oil untill 130°C ... you will smell some kind of sweet chestnut-like fragrance. Than you know your fb is done.
After letting it cool. You can add the aceton, than the HCL to level up the PH.

I normally put it in the fridge and let it cool untill -30 degree. But that is my methode.

I read that your fb smells like rotten fish. Well that is the mixer of methanol and your methylamine. Your fb should smell almost like nothing at the end. At least some kind of chestnut fragrance.

Not adding enough water to clean your fb will make your crystal's look brownish at the end. (You can do this in parts if you don't have a bigger reactor, or calculate your mixture before making a large portion out of it so it all fits in your reactor.)
 

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chestnut fragrance - exactly, bro!!! light beautiful smell of chestnut
 

Pororo

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mdma fb oil is always heavy. it's density is exactly 1.1g per 1cm3. so it always stay below water if no any inorganic compounds (NaCl for ex) is dissolved in water.
 

Pororo

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I may not understand all your text properly, but if you add some alcohol or acetone in your base + dcm + water system, then alcohol or acetone will go to both: top water layer and lower dcm layer.
At the same time, some part of base will go to top (water) together with alcohol, and some part of other compounds soluble in water will go to dcm layer. And this is a disaster!!!

I also do not like dcm, as it has pretty high solubility in water if compare with other similar solvents. DCM is not right choice.
 

CCL4 huffer

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erm mate if u add dcm to water it will always go to the bottom
 

Pororo

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erm mate, did I say dcm is miscible with water? i said dcm has maximum solubility in water among other non-polar solvents. also dcm, due to its chemilac and phisical structure solves a lot of polar compounds insoluble in other non-polar solvents such as ether, hexane, perc etc.
 

togeter

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@lucas_cash but i already did vacuum distilation to get the freebase at 160c, there is any chance that i still get methanol with methylamine to my freebase?

Can anyone give me a safe method to work with methylamine next time, because people say methylamine is very toxic
 

CCL4 huffer

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@Pororo wasnt replying to u was replying to that dude that said if u do everything right it will go to the bottom witch dcm always will with water
 

lucas_cash

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Did you read my text correctly. I never said you add all these things together at once. There are steps in between. also did you ever make mdma? If not, than u don't understand what is been saying here. If you did make it. Then you know dcm is never used with acetone in this case. And only a small amount of dcm is used to separate the oil that you need from the rest of the water and whatever is in it....
 

lucas_cash

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If you vacuum distilled it. Then your oil should have stayed in your reactor and the rest should have evaporated or captured it into an other flask.

So if you took the colorless liquid and continued working with that. It means you took the wrong one, which had the methylamine in it. That is why you kept smelling it. because fb is never colorless.

Did you turn your pmk wax into pmk oil?
Dm me if you want.
 

NucleuZ

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