4-MMC synthesis

Berlin777

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Yeah the first ones looked very dirty, I only showed them to compare to current ones, which are cleaner, I am aware of mistakes which I’m trying to fix, ordering few things to improve production and quality.

If you can safely ship MA40% to the UK I will be happy to buy it.
 

Berlin777

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It’s cleaner compared to my first batches
 

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$!$

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After some failures due to my lack of patients finally got some good results thanks to @William Dampier @Marvin "Popcorn" Sutton and passive spectator @G.Patton

My first batches were pretty shit because I rushed too much and didn't use appropriate equipment. For instance I used 250ml drip funnel and I waited only for couple of minutes for the layers separation because I wanted to finish asap and that was the result (1st picture) , I'm gonna blend it, rinse it and crystallize it.
For the first batches I used BK4 and MA40%

After few fuck ups things started getting better, recipe changed a little bit because there are some issues with MA40% but I feet comfortable with current method.

Current method is cold synthesis, works good for me:
500g BK4 is dissolved in 1500ml DCM in 6L flat bottom flask using magnetic stirrer
500g of NaOH is dissolved in 1L H2O cooled (about 10 C) down and added to the flask
750g MA HCl is added to the flask in small batches so the temperature doesn't raise too much, roughly 100g - 150g every 10-15 minutes
The lid is closed and it's left for 16 - 24h hours on the stirrer

After that salt has to be filtered with buchner funnel, then the layers separated prepared for washing.
For first washing I use 3L filtered water with 150g sodium bicarbonate heated up to 30 C
Second washing just 3L of filtered water.

Once it's washed I use about 160ml and 800ml acetone for acidification and to get mephedrone powder, once pH 5 or lower is reached I put it to the freezer and leave overnight.
On the next day I filter as much as possible and leave it to dry. When I skipped that and filtered still wet mephedrone the yield was 240g, yesterday I done it Marvins way and it was 258g.
Marvins way
1. Filter
2. Dry
3. Rinse (cold acetone)
4. Dry
5. crystallize

Crystallization
1:2 powder mephedrone to water and alcohol 50% of the amount of water

I just pour the water to the pyrex glass bowl add mephedrone heat it up until little bubbles appear, boil for 5 minutes, switch the heating off and add alcohol the pour it to the crystallization dish and wait.

So if we compare how it stared and how it's going it's a big difference.
Berlin777Hello boss.
How much gram you get when crystal was dry ??
I'm say crystals no powder
 

Berlin777

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Hello boss.
How much gram you get when crystal was dry ??
I'm say crystals no powder
$!$I don't check it anymore to be fair because the last batches of crystals are not pure enough to sell them so I wait for complete evaporation then purify whats left. Now I had about 400g ground and purified crystals from several batches.
 
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I don't check it anymore to be fair because the last batches of crystals are not pure enough to sell them so I wait for complete evaporation then purify whats left. Now I had about 400g ground and purified crystals from several batches.
Berlin777i see u are use methyloamine hcl and u made your self monomethyloamine
with NaOh and water i made like you say up ??
 

Berlin777

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i see u are use methyloamine hcl and u made your self monomethyloamine
with NaOh and water i made like you say up ??
$!$Gas is released in reaction flask after adding MA HCl. I am not sure what's your question.
 

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Gas is released in reaction flask after adding MA HCl. I am not sure what's your question.
Berlin777To get 1l methyloamine 40% in water you use
500g NaOh
750 methyloamine hcl
and 1l water ??
 

Berlin777

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BK4 to MA HCl ratio is 1-1.5
I don’t use water, I don’t make 40% solution. Methylamine gas is released in RM with help of NaOH solution.
 

Berlin777

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BK4 to MA HCl ratio is 1-1.5
I don’t use water, I don’t make 40% solution. Methylamine gas is released in RM with help of NaOH solution.
Berlin777and it's better to use a little bit more water for NaOH solution so RM won't heat up that much while adding MA HCl
 
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