4MMC Reagent Kit - First Synthesis (100g Scale)

[Gordon Ramsay]

4MMC Synthesis Report (100g 2B4MP)

1. 100g 2b4mp was placed inside of a RBF and 350ml of DCM was added. The solution was stirred for approx. 5 minutes, untill the 2b4mp was fully dissolved in DCM
2. 200ml Methylamine 40% was added in 3 portions (70ml, 75ml, 55ml), every 15 minutes. The temperature started to rise towards 28-30 °C, the colour started to turn slightly yellow
3. The temperature was set to 63 °C so that the RM could reach a temperature of 40°C - 38°C, on the top the temperature remained 30 °C, we assume it is because of the aeqeous layer which already started to form there

4. After 2h of synthesis, 500ml of DH20 was added and allowed to stirr for 5 min. The solution was given 20 minutes to seperate layers, The washing procedure was repeated a total of 4 times, organic layer was kept to proceed.

5. Approximately 175ml of DH2O was added to the previously obtained Meph-Oil (300ml). Stirrer was turned on so that the layers will not seperate

6. ph 5 was reached and the solution was set aside to sepeate layers. The top layer was decanted, the ph of both layers was confirmed.

7. 150ml of Isopropyl 99% have been added to the aeqeous layer of the acidified solution and the solution was heated to 70 °C until slight boiling bubbles showed, the solution was put inside of a glassware dish and locked in a shelf (dark & sealed). Crystalization will take approximately 5 days and the report will be completed once the crystalization was completed.

8. The remaining DCM layer was put into the freezer for 10h as 4MMC remained inside of the DCM layer, when removed a layer of crystals has formed on top (wet weight: 18.41g). It will be put aside for later processing and to learn recrystalization of 4MMC.

 

[Gordon Ramsay]

Thanks a lot to @William Dampier and @Marvin "Popcorn" Sutton for the help during the process.

The next batches will be with increased volume and focused on purification methods to remove excess smell fo Methylamine and also water residues inside of the acidified aeqeous layer, additional crystalization methods will also be tested.

 

[xoxoxoxo]

Picture cant see

 

[Gordon Ramsay]

Picture cant see

xoxoxoxoMaybe try to reload

 

[PsychedelicDog]

Maybe try to reload

Gordon RamsayThe images are uploaded to the tor website they can only be viewed there.

 

[Gordon Ramsay]

The images are uploaded to the tor website they can only be viewed there.

PsychedelicDogMakes sense

 

[xoxoxoxo]

u get 11g dry 4mmc hcl forom 100g 2b4m?? yes xD

 

[Gordon Ramsay]

u get 11g dry 4mmc hcl forom 100g 2b4m?? yes xD

xoxoxoxoThe solution is waiting to crystalize 18.41g wet crystals was from the DCM layer, so secondary batch of crystals.
I expect the main batch to be more

 

[Jackson]

great job but the pictures aren't loading.. they are too big.

 

[Gordon Ramsay]

great job but the pictures aren't loading.. they are too big.

labrat23Thank you Do you maybe see something that could be improved?

Once I have learned more about crystalization and also about a larger scale of at least 3kg 2B4MP, I will upload an extended report to the main forum section for Methcathiones

PS - you can open the pictures in a second tap to load them

 

[Jackson]

I am no expert I don't know how you could improve.. maybe make a vid after a few tries

 

[Jackson]

only last picture is visible.. i tryed from pc and phone but no luck.. can' right click and view image or nothing..

 

[xoxoxoxo]

View attachment 23192

only last picture is visible.. i tryed from pc and phone but no luck.. can' right click and view image or nothing..

labrat23made crystals is very easy to made.
proportions of reagents, then start heating, these are just the basics, there are many experts here, simple molar calculations, basic chemistry. there is a table which solvent needs to be heated, how much it needs to be heated and what is its time freebase purification sometimes it may happen that 2b4m will not react with methylamine and it needs to be cleaned well. Likewise, freebase cannot be overheated because it will start to precipitate by-products such as pyrizine, methylenepropiophenone or bromine residues. if your efficiency is 10% 40% 50% then it is very low, the maximum value is 95% as described Hank Schrader. the same crystallization can be done in 2 days or 2 weeks

 

[Gordon Ramsay]

Crystalization will take approximately 5 days and the report will be completed once the crystalization was completed.

Gordon RamsayUpdate on the crystalization process:

 

[Jackson]

is it still liquid in the middle?

 

[Gordon Ramsay]

is it still liquid in the middle?

labrat23Yes, crystals are growing from bottom and top in this case I have not expected it like that but it looks cool!

 

[Jackson]

this is after you left it at room temp (~24*C) for 6 days right?
would it be faster if you leave it in refrigirator?

 

[Gordon Ramsay]

this is after you left it at room temp (~24*C) for 6 days right?
would it be faster if you leave it in refrigirator?

labrat23Yes exactly

The room is not ideal, high humidity and flucuating temperature as there is work done in the same room.
Next time I will do it in a dedicated room with an air dehumidifier or temperature controle

Crystalizing in a freezer will be faster but I want to try different methods. My main method is using the rotary evaporator, it is very convenient!

 

[Jackson]

Step 5: Crystallization

Dissolve 50g of pure mephedrone powder in 100ml of water (or 50/50 alcohol water or vodka). Heat until bubbling and allow to crystallize in a bowl. You will get mephedrone crystals after the solvent evaporates

did you not try this way?

 

[Gordon Ramsay]

Step 5: Crystallization

Dissolve 50g of pure mephedrone powder in 100ml of water (or 50/50 alcohol water or vodka). Heat until bubbling and allow to crystallize in a bowl. You will get mephedrone crystals after the solvent evaporates

did you not try this way?

labrat23150ml of Isopropyl 99% have been added to the aeqeous layer of the acidified solution and the solution was heated to 70 °C until slight boiling bubbles showed, the solution was put inside of a glassware dish and put away to crystalize.

This is what I have done exactly.

It is necessary to heat the resulting aqueous solution to a temperature close to boiling. Add to the hot aqueous solution ethanol in the amount of 1/3-1/2 of the volume of the aqueous solution. Pour into a Pyrex glass dish so that the liquid layer is 5cm and leave in a dry place at room temperature.
You can use air conditioner or dehumidifier to accelerate crystallization.
To make the crystal grow long needles, the solution must not be disturbed or stirred.
Usually a microclimate cabinet or racks are used for crystallization. This requires a constant temperature and dry air.

This is my general guide by @William Dampier and @Marvin "Popcorn" Sutton

Large crystals will be good for your marketing and for the pleasing of your customers eyes. But small fractions obtained from the rotary evaporator will be best for your consumers and also for you to handle them. They are obtained by evaporating water & remaining liquids from the acidified aeqeous layer using a rotary evaporator,

I will update the post here aswell

 

[Gordon Ramsay]

4MMC Synthesis Report (200g 2B4MP Scale)

For todays synthesis the scale was increased to 200g 2B4MP, we simply doubled the volume of each reagent.
Todays target was to obtain salt like 4MMC HCL crystals directly from the rotary evaporator

Reagents

2B4MP 200g
Methylamine 40% aeq. 400ml
DCM 700ml
Distilled Water 3.950ml
HCL 37% ~90ml

Equipment

2.000ml RBF
Heating Plate & Magnetic Stirrer
Rotary Evaporator
Glassware

1. 200g 2b4mp was placed inside of a RBF and 700ml of DCM was added. The solution was stirred for approx. 5 minutes, untill the 2b4mp was fully dissolved in DCM

2. 400ml Methylamine 40% was added in 2 portions (each 2x100ml), every 20 minutes. The temperature started to rise towards 28-30 °C, the colour started to turn slightly yellow

3. The temperature was set to 63 °C and the lask completely wrapped in aluminium foil so that the RM could reach a temperature of 40°C - 38°C. Once reached, it was stirred and cooked for 2h, the tone of yellow got stronger

4. After 2h of synthesis, 900ml of DH20 was added to wash the obtained meph-oil and allowed to stirr for 5 min. We gave it 20 minutes to seperate layers
The washing procedure was repeated a total of 4 times (2 times is enough), we kept the organic layer containing Meph-Oil on DCM and proceeded.

5. Approximately 350ml of DH2O was added to the previously obtained Meph-Oil/DCM solution. Stirrer was turned on so that the layers will not seperate to drip the solution down to PH=5 with HCL 37%.

6. ph 5 was reached and the solution was set aside to sepeate layers. The top layer was decanted, the ph of both layers was confirmed to be ph=5.

7. The remaining DCM layer was put into the freezer for later processing

8. The acidified aeqeous layer is ready for a rapid crystalization in the rotary evaporator. All liquids got evaporated to yield a sugar sized salt

9. The salt obtained from the rotary evaporator was removed from the distillation flask and cleaned with ice cold Acetone, using a Buchner funnel and vacuum to get rid of impurities. Yield wet: 152.01g

 

[xile]

4MMC Synthesis Report (100g 2B4MP)

1. 100g 2b4mp was placed inside of a RBF and 350ml of DCM was added. The solution was stirred for approx. 5 minutes, untill the 2b4mp was fully dissolved in DCM
2. 200ml Methylamine 40% was added in 3 portions (70ml, 75ml, 55ml), every 15 minutes. The temperature started to rise towards 28-30 °C, the colour started to turn slightly yellow
3. The temperature was set to 63 °C so that the RM could reach a temperature of 40°C - 38°C, on the top the temperature remained 30 °C, we assume it is because of the aeqeous layer which already started to form there

4. After 2h of synthesis, 500ml of DH20 was added and allowed to stirr for 5 min. The solution was given 20 minutes to seperate layers, The washing procedure was repeated a total of 4 times, organic layer was kept to proceed.

5. Approximately 175ml of DH2O was added to the previously obtained Meph-Oil (300ml). Stirrer was turned on so that the layers will not seperate

6. ph 5 was reached and the solution was set aside to sepeate layers. The top layer was decanted, the ph of both layers was confirmed.

7. 150ml of Isopropyl 99% have been added to the aeqeous layer of the acidified solution and the solution was heated to 70 °C until slight boiling bubbles showed, the solution was put inside of a glassware dish and locked in a shelf (dark & sealed). Crystalization will take approximately 5 days and the report will be completed once the crystalization was completed.

8. The remaining DCM layer was put into the freezer for 10h as 4MMC remained inside of the DCM layer, when removed a layer of crystals has formed on top (wet weight: 18.41g). It will be put aside for later processing and to learn recrystalization of 4MMC.

View attachment 23144

Gordon RamsayI thought it dosent have to be recrystalated? Your product Look like mine, but it seems like your product is a little dirty. I reach it by toulene. Dcm synthesis never work for me.

Toluene is far easyer since the organic layer remains in separation funnel and with acidify by Aceton give back a realy clean produckt.

After drying you are able to recrystlize imediately.

 

[Gordon Ramsay]

I thought it dosent have to be recrystalated? Your product Look like mine, but it seems like your product is a little dirty. I reach it by toulene. Dcm synthesis never work for me.

Toluene is far easyer since the organic layer remains in separation funnel and with acidify by Aceton give back a realy clean produckt.

After drying you are able to recrystlize imediately.

xileWhen it is coming out of the rotovap, it is dirty I then flush it with frozen acetone one time to let it dry up. Once dried I will clean it further to have a perfectly clean product

What do you mean with recrystalization? I have not recrystalized yet

What was your issue with DCM?

 

[xile]

When it is coming out of the rotovap, it is dirty I then flush it with frozen acetone one time to let it dry up. Once dried I will clean it further to have a perfectly clean product

What do you mean with recrystalization? I have not recrystalized yet

What was your issue with DCM?

Gordon RamsayI can't manage to separate the layers with dcm. I've never had product at the end. With toluene I got the same result as you. But my instructions never mentioned using powder first. It was said that the removed dcm layer (below) is diluted with 100 ml of water and acidified. At ph5, stir vigorously and adjust the ph again. The upper layer of water is then removed and placed in the crystallization dish. According to these instructions you don't get a white or dirty powder, but a viscous brown mass.

Since there is so much color in there I think I didn't separate it properly. But it's too expensive for me to continue working on a method that hasn't achieved anything so far, even though I know a method that I've already successfully used to produce a product.