4-MMC (mephedrone) synthesis. Complete video tutorial.

[malignoalfa]

CH3NH2·HCl (67.52g) + NaOH (40g) → CH3NH2 (31.06g) + NaCl (58.44g) + H2O (18.01g)


200ml of 40% aqueous methylamine => 80g CH3NH2 dissolved in 200g H2O



If I use (174g of methylamine hcl + 67% aqueous NAOH solution)

CH3NH2.HCL 174g
NAOH 103g + H20 154g

I obtain (200ml of 40% aqueous methylamine):

CH3NH2 80g
NACL 150g
H20 200g

Would it be possible?

 

[malignoalfa]

REAGENTS

CH3NH2·HCl 67,518 g/mol
NaOH 40 g/mol


PRODUCTS

CH3NH2 31.0571 g/mol
NaCl 58.4428 g/mol
H20 18 g/mol


I decided to do some calculations myself to clarify the matter for myself; maybe it will clarify for others.

Methylamine aq 40% → 1 CH3NH2 (31g) + 2.5 H2O (45g)


31g divided by 31g + 45g = 40%

The density of Methylamine 40% (w/w) in water is 0.897 g/mL, that is, 200ml has 179.4 grams.

40% methylamine = 71.76g (2.31 mol)
60% water = 107.64g

I have seen recommendations to use a 1:5 ratio of NaOH to H2O and add dropwise to an ice bath aqueous solution of methylamine.hcl. Perhaps the use of a lower concentration of NaOH for basification has the objective of making the reaction more peaceful, not heating, not releasing methylamine in gas; but I can't say for sure.

To clarify, the 1:5 ratio of NaOH to H2O refers to a 31% concentration.

1 mol NaOH => 40g
5 mol H20 => 90g

40g divided by 40g + 90g = 31%

Methylamine.hcl has a water solubility of 1g/mL (at 20 °C)
1 mol CH3NH2.HCL => 67.52g would need 4 mols of H20 (72g/72ml) to completely dissolve, a concentration of 48%:

67.52g divided by 67.52g + 72g = 48%

The balanced reaction equation is:

CH3NH2·HCl + NaOH → CH3NH2 + NaCl + H2O

The equation involving solutions of methylamine.hcl with NaOH solution above would look like this:

(1 CH3NH2·HCl + 4 H2O) (48% aq) + (1 NaOH + 5 H2O) (31% aq) → 1 CH3NH2 + 1 NaCl + 10 H2O

To obtain 2.31 mol of methylamine equivalent to 200ml of Methylamine 40% (w/w) in water, we would have:


(2.31 CH3NH2·HCl + 9.24 H2O) (48% aq) + (2.31 NaOH + 11.55 H2O) (31% aq) → 2.31 CH3NH2 + 2.31 NaCl + 23.1 H2O

In grams, we would have (rounded):

(156g CH3NH2·HCl + 166g H2O) + (93g NaOH + 208g H2O) → 72g CH3NH2 + 135g NaCl + 416g H2O

We would have 72g of methylamine with 135g of NaCl dissolved in 416g (ml) of H20.
An aqueous solution of 33% methylamine + NaCl, being 11% methylamine and 22% NaCl.

72g + 135g divided by 72g + 135g + 416g = 33%

72g/623g (11%) + 135g/623g (22%) = 33%

I don't know if excess water would disturb the synthesis of this topic, but just removing excess water with a drying agent without removing NaCl would not solve it, as we would have solubility problems (maximum saturation). I couldn't tell if the NaCl would precipitate or if the methylamine would be released as a gas, or perhaps both.

 

[aa1178251182]

Did you synthesize 4-MMC with methylamine hydrochloride?

 

[Chery]

Why is no one using methylamine in methanol, i thought an anhydrous medium would increase the yield?

 

[bonotuto]

This is cooll man...youre awesome teach us with completed video tutorial...cherrsss

 

[OttoBulletproof]

Can Methylamine HCL be used or does it have to be Freebase?

 

[UWe9o12jkied91d]

has to be freebase, just mix hcl with naoh

 

[chuckmcgill]

do you have a good formula for making 40% aqueous methlyamine from its HCL and NaOH? I tried based on a technique in here that uses 40g methylamine HCL in 100ml water mixed with 17g Naoh in 50ml water. That seemed to not produce satisfactory results. The molar ratios seem off too but the poster said it is the only ratio he found to work

 

[cartelloszetas]

My mmc thanks bb forum for help. U are the best ✓

 

[UWe9o12jkied91d]

Superb, care to share more on method used for recrystalization?

 

[tajira]

Can someone confirm these proportions for 100g of 2Bromo4Methylpropiophenone
2Bromo4Methylpropiophenone - 100g
DCM - 300ML (3ML PER G)
NMP - 300ML
METHYLAMINE - 200ml

 

[cartelloszetas]

Made and u will see is true or not

 

[HerrHaber]

It may well work but the whole thing comes with practice thus don’t jump into big quantities (100g is ok if you have the other 900g left).

 

[Mephisto]

Hello, I have a problem. I tried the synthesis in various ways, on NMP extracting with teluene and ethyl acetate, on acetate only, almost always with an excess of methylamine. Usually it is possible to collect freebase well from the primary mixture using extraction, sometimes the problem is with extraction with ethyl acetate with water alone, sometimes it can not separate after animation, especially when it is used for extraction from RM on NMP, toluene as a typical nonpolar solvent for example picks up the freebase from NMP RMs well, which in turn is well miscible with water, so I think it can be considered the most efficient solvent for this reaction, NMP i mean. In syntheses, they usually describe that you need to heat RM on NMP for 40 minutes, but due to the miscibility with water, it can be assumed that the reaction proceeds here even faster and more efficiently than on ethyl acetate. It is also known that the reaction is exothermic, so when the temperature starts to drop, the reaction is theoretically over. Okay, but still my problem is that how would I not do it when acidifying, salt does not want to show up, I drop acid to pH 5.5-6, mix and mix and nothing, possibly darkens, but nothing it does not precipitate, and it should have swelled and become thick a long time ago. If such a mixture is then given for cooling or evaporation, nothing appears, only possibly black tar is made. And so practically every time. Recently, I just figured out that there is some sediment as after acidification I add some alkali like baking soda or caustic. Why is that, can someone help me solve this puzzle and tell me what I'm doing wrong?

 

[UWe9o12jkied91d]

List the steps taken succinctly, in order if you want a good answer.
Check your methylamine, it might steel reek to your human nose but it might be 15%.Percentage HCl used? Dried freebase before acid? Used acetone(cold) 1:1 in relation to rm+extraction solvent?Forgot about an acidified portion for 2 weeks in the back of the freezer? Kissed your cousin?

 

[Albert A]

Hello everyone, Can someone please explain to me why the methylamination reaction is made simultaneously in two solvents benzene and NMP ?
(Not in one solvent).

 

[PolandoEmingarnte]

because u made 2b4m and then 4mmc

 

[Albert A]

I can melt dry 2-Bromo-4-Methylpropiophenone in NMP and then do methylamination?
it will be OK?

 

[PolandoEmingarnte]

u can of cours

 

[marty€mcfly]

I’m producing a yield today and I thought it’ll be helpful to give give an old method I used in my beginning stages as a chemist. It’s a simple method I’ve found for beginners and you don’t need much equipment.

Synthesizing commercial simple 4-bromoketone.

I will use methylamine in 40% aqueous solution w/ dcm for a simple Nucleuphile with Sn2 substitiotion.

2bromo4methylpropiophenone, dcm, and 2.5x moles the equivalent of methylamine needs a really good stir while keeping a constant cool temperature with an ice bath.

After the third addition remove the ice bath and stir for 6 hours more while keeping a constant room temperature. Here will be noticed a layer turn from yellow-dark yellow-orangish.

Next add a precooled solution of NaOH until it reaches 11 ph.

Adding cooled sodium hydroxide into the solution, this will cool the natural thermal effects and preserve the proper reaction process.

Maneuver a water hose like device with hydrochloric acid solution to recycle some methylamine.

Give a good wash 2-3 time with brine solutions, and extract with aqueous diluted hydrochloric acid.

Wash off acidic layer with toulene and evaporate to obtain white crystalish powder consistant uniformed product. Next carefuly extract with vacum about 3-4 times with chlorofom, then evaporate the cholorofm to obtain the pure mephedrone. You can disolve it in hot IPA/water and let it evaporate slowly, it will create small crystals.

It can be also be obtain better with dibenzoyl-I-tartaric acid to resolute the reacemic mixture but think it’ll be easier for beginners with the first mechanism using IPA.

With dibenzoyl-I-tartaric acid you will have to add portions 1:1 mole of the acid per mole of amine in ethyl acetate and salt will precipitate. Then just follow up carefully with some A/B to obtain between 70-90% enantiomery pure mephedrone.

“You absolutely have to acidify the finished product with isopropanolic/hcl in order to react it because heating cathinones with acids racemizes them”.

 

[PolandoEmingarnte]

after 1 you can do the synthesis much faster, easier and you don't need labo equipment at all. synthesis can be done in 1.5 hours tartaric acid haha probably hydrochloric acid. no need to use ipa acetone or ethyl acetate in the synthesis. You write for a beginner where you have how much what do you have to add there is no freebase cleanup at all and naoh only burns freebase is another thing.

 

[marty€mcfly]

I have access to a lab & lab equipment now so, h don’t use it anymore but, it’s nice to share!

 

[Albert A]

How did the prescription change under more favorable conditions in the lab?

does the type of solvent ( DCM or NMP) if keeping the heat limit not affect the cleanliness of the final product?

 

[Albert A]

what is the difference between them?

 

[marty€mcfly]

I can’t say what changes the color chemically because I could be wrong but each solvent needs a different care. I just know the methods I use, and keeping a constant temperature with an ice bath keeps the color light.

“I can’t say that the lab makes it better because I’ve struck gold in less professional settings”. I -can-recant-that!