Shake and bake method for 4mmc

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Chemicals
{100g}
2-bromo-4methylopropiophenone
{500ml} dcm toulen or benzen
{200ml} methyloamine 40% in water
{3x300ml} cheap water from shop with no gas!!!
{500ml} acetone technical from the construction shop
{55ml} acid hcl 35%-38% if you have 31% acid then we need more to use
This all what we need to made this way:)
 

ymaaah

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U said "cheap water from shop" but u dont need to use distillate water? Demineralized water can be good?
 

41Dxflatline

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Drinking water is usually reverse osmosis and UV decontaminated.
 

StarWars

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Video shake and bake

 
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HerrHaber

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I am still opting for the conventional chemistry way
 
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HerrHaber

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I worked a lot with alpha halogenated ketones in University lab and lachrimatory effect was always a problem... I know why it is worth it because I am also well aquainted with the mephedrone high so thumbs up!
 

StarWars

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There need also wash water with soda and later 3x water and extraction with dcm and later need use magnesium solfate and last step with acetone and acid
 

ymaaah

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I have a question, why he takes the top part of the solution to heat it? the bottom part is 4mmc freebase so why he takes the top part?
 

byczyborsuk

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Hi. 200 ml 9% 2-bromo-4methylopropiophenone mean that i need 182ml of water mixed with 18 gram of 2-bromo-4methylopropiophenone or different weight and i have to use other solvent ?
How you sorting out metylamine and HCl in one pot method?
 

HerrHaber

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A brief translation of what is going on in the video may help... it's just curiosity
 

ymaaah

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whats the yield? Not a lot I imagine..?
 

StarWars

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Made u will see
 
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ymaaah

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what does it mean? :)
The yield is bad? :)
 

StarWars

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Made u will see how much u get.
 

breathing.fire

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Somebody know if this reaction come with methylamine 33 % in methanol
 

StarWars

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No only with metyloamine with water
 

RegulierTier

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Ok, did I understand this correctly?

Step 1: Two solutions are prepared:
Solution 1: 100 g of 2b4m are dissolved in 500 mL of DCM
Solution 2: 200 mL of a 40% methylamine solution

Both solutions are combined in a container, which is then sealed and shaken for 30 minutes.

Step 2: Approximately 200 mL of water is added to the mixture and shaken.
The aqueous phase is discarded. This step is repeated 2-3 times.
The lower phase now consists of DCM and 4-mmc freebase.

Step 3: A solution is prepared consisting of 55 mL of HCL and 500 mL of acetone.
This solution is added to the dcm/4-mmc mixture until the pH level reaches 5.5-6.0.

Step 4: The solution is evaporated until the 4-mmc precipitates out as a salt.
 

HerrHaber

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the hydrochloride should precipitate upon acidification, and partial evaporation is inevitable but I'm not 100% sure you should waste your time trying to evaporate (rather concentrate) the suspension, instead place it in the freezer for some hours and then filter it, you are advised to let the filtrate (remaining liquid) evaporate some more then freeze again for a second crop of lesser quality (considering everyone wants to see them big crystals recrystalization is a must, you can combine the solids or recryst separately if the second one has an obvious drop in quality)
 
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mocnykutas

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you can add all the methylamine at once it's nonsense you don't have to add it for an hour xD
 

RegulierTier

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I have 2 questions. The first question is: I don't quite understand the purpose of the bag. What is it for and how do I attach the bag? The second question is: Can I also use methylamine hydrochloride and prepare the solution according to the following calculation, so that I dissolve 0.2487 g of methylamine hydrochloride in 200 mL of water?
Provided I haven't miscalculated or made a mistake somewhere in my thinking.

CEofPpeFj8
 

HerrHaber

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Your calculations are presumably correct but you still need to freebase the methylamine hydrochloride to obtain an aqueous solution of methylamine that will also have the alkaline chloride (Na in case of NaOH and K in case of KOH) in equimolar amount therefore your aq solution will be to the same extent methylamine and Alkaline chloride (the percentage of methylamine in that water can't possibly be 40% since there is an equal amount of say NaCl).
The bag question is a silly one but I'm feeling you why it got you confused, the jar may not be completely sealed by it's own lid alone so the purpose of the bag placed in between the top of the jar and its lid is to form a tighter seal so that the MeNH2 gas can not escape the reaction enclosure, for the same reason people also put tape around the closure.
I hope this is disambiguating rather than further complicating things for you. Feel free to ask for more detailed explanation and I promise to do my best to explain it all over again which is better than you doing misstakes.
Cheers!
 
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