Need help please making 4mmc, just some guidance

[white7proton]

My old profile is ThisIsMyName but I lost all my log in info and I can't remember it! I paid for the highest membership as well so I'm gutted.

I've tried to make 4mmc powder today from 2b4m, I tried only step 1 list and I feel like I messed it up, something wasn't right and I don't know what. I need help with the method if possible please, once I get it I will be fine its just initially getting it into the brain of mine.

The ingredients I used were the following:

STEP 1
2b4m 100g
Dcn 500ml
Methyloamine 40% in water 200ml
3x water 200ml
Dcm 200ml with 5% soda
Later drop 1g NACI
Acid 55ml and 500ml acetone

STEP 2
1g 4mmc
2ml water
0.5 ml ipa alcohol
Or wodka pure from shop 40% pure
3mgvitamin c ascorbic acid

Please someone help me

 

[HEISENBERG]

Hello
Hello. Contact me so I can restore your access to your old account. If you need help with 4mmc synthesis, you can ask @G.Patton, he will not refuse to help you.

 

[white7proton]

Okay. I'll message you later. I'm just at work, that's wicked if you can help me get my account back. My Russian encrypted phone had that account on and the phone is missing so lost all my info unfortunately.

 

[G.Patton]

Hello, can you describe in details your synthesis and problems? Nobody can help you without it.

 

[white7proton]

Yes I'll write down what I did. Just at work, when I am home ill explain it simply exactly what I did.

Just give me a few hours, thanks for the replys

 

[white7proton]

Safety equipment:
Gloves
Gas mask

Stage 1

1. Add 100g 2b4m and 500ml dcm put in large glass bottle (1.5l vodka bottle), shake until all dissolved (10 minutes)
2. Add Methyloamine 40% in water 200ml to bottle in 3 parts, shake after each part added. Seal glass bottle with lid, use electrical tape and wrap the lid tight and seal completely.
3. Shake bottle every 10 minutes for 30 seconds over the course of 2 hours.

1st photo is 2b4m and dcm
2nd and 3rd photo is 2b4m, dcm and 40 methyloamine added and sealed.

I'm doing this right now. So what will step 4, 5 and 6 etc be please.

 

[white7proton]

Will leave in bottle for 2 hours and shake every 10 minutes.

Next steps i will add the following:
3x water 200ml
Dcm 200ml with 5% soda
Later drop 1g NACI
Acid 55ml and 500ml acetone

Can you guide me on these steps please

 

[white7proton]

So shortly I will take out and discard the top layer of the mixture as shown in the photo.

Then I will wash the lower part of the mixture 3 times with 200ml water then I will discard the water part of the mixture after each wash

What do I do with the 200ml dcm with 5% bicarbonate soda?

 

[white7proton]

I believe I need to add the dcm and bicarb to help extract as much 4mmc as possible, then I will mix 55ml and 500ml of acetone together and slowly add this to the mixture.

How slowly or how much at a time do I need to add to prevent burning the mixture?

 

[G.Patton]

You can use DCM to extract water layer to collect all 4-mmc residues. I have no idea where did you take this recipe with bicarbonate soda.

You have to combine dcm layers and add acetone/hcl mixture there

 

[white7proton]

Once I have added the acid to the acetone I will then add this to the mixture, how long before the chemical process is completed?

I add the salt NACI before adding the acid and acetone.

How do I get the 4mmc from this mixture? I don't have a vacuum machine to extract the moisture and leaving me with the powder, is there another way to do this? Can I not just add acetone straight to this instead of making powder? So I can crystalize quicker skipping this step?

Once I have perfected this 100g 2b4m recipe and method I will tryand do 1000g 2b4m, but I will need to do it in a way where I use normal equipment and normal containers not laboratory equipment.

 

[G.Patton]

Depends on reaction volume, until precipitation is stopped. You have to reach 5.5-6.5 pH.
What is a reason? There is no sense.
filter 4-mmc crystals via filter paper in case you don't have suction filtration tool. Then, air dry them. That's all.

 

[white7proton]

I'm going to take the top layer off this mixture now, in the photo is 100g 2b4m, 500ml dcm and 200ml methyloamine 40% after 2 hours of reacting and shaking every 10 minutes.

I'm going to take the top layer away and discard it. Then wash it 3 times with 200ml water, so 600ml total until the methyloamine smell goes. I may wash even more times.

 

[white7proton]

I have taken top layer off

 

[white7proton]

Added 200ml dcm 5% bicarb soda and 1g NACI

 

[G.Patton]

Why did you do this? What is a purose of this step, can you tell me please?

 

[white7proton]

Now I will mix 500ml acetone with 55ml hydrochloric acid 35/36.6%

Then I add this to the main mixture.

This is what it looks like after I add the 500ml acetone with 55ml hydrochloric acid 35/36.6% bit by bit..

 

[white7proton]

That's what it looks like after acetone and acid being added...

 

[G.Patton]

Please, stop flood here. Write in one message or in direct message me.

 

[G.Patton]

Looks that you've overoxydize your 4-mmc. What pH do u have?

 

[HEISENBERG]

Don't rush to post everything. Think about it and write once.

 

[hexen]

My. 4-mmc HCl

 

[white7proton]

What have I done wrong? I don't understand.

 

[white7proton]

Mine has gone all dark instead of creamy. Can you let me know your opinion please.

 

[hexen]

What pH u have ?

 

[white7proton]

Hopefully tomorrow when I put the mixture through the filter I get powder. If I don't get any powder then I don't know what I am doing wrong.