Need help please making 4mmc, just some guidance

[white7proton]

Stage 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

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.
4. Next take the top layer away and discard it (lighter in colour).
5. Then wash it 3 times with 200ml water, so 600ml total until the methyloamine smell goes. I may wash even more times. Discard the water after each wash.
6. Add 200ml dcm 5% bicarb soda and 1g NACI to the main mixture.
7. Now I will mix 500ml acetone with 55ml hydrochloric acid 35/36.6%, then I add this to the main mixture bit by bit.

My mixture is all dark after doing the above... what have I done wrong please?

 

[G.Patton]

There are several mistakes:
1. Why do you add 200 ml 5% bicarb into the reaction mixture
2. You had to dry your solution over Na2SO4
3. You added too much acid (I guess), cuz your product had too dark color.

I don't know where did you take this and don't uderstand why it is hard to open video synthesis tutorial for you. In the BB Forum several correct manuals.
I already answer above to your questions. Please, ask all your next question in one message, no more. You overflooded this comment section and made it not readable for other users and for me.

 

[white7proton]

Ingredients and Measurements:

• 2-Bromo-4'-methylpropiophenone (cas 1451-82-7) - 100g
• DCM - 400ml
• Methyloamine 40% aq. solution (cas 74-89-5) - 160ml
• Distilled water - 400ml
• DCM - 400ml
• Acetone - 600ml
• Hydrochloric acid con. aq. solution (HCl 36%) ~ 30ml

1. Add 100g 2b4m and 400ml dcm put in large glass bottle (1.5l vodka bottle), shake until all dissolved (10 minutes)
2. Add Methyloamine 40% in water 160ml 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.
4. Then wash it 2/3 times with 400ml water total, until the methyloamine smell goes. I may wash even more times. Discard the water after each wash.
6. Add 400ml dcm.
7. Now I will add 600ml ice cold acetone to the mix.
8. Add 30ml hydrochloric acid 35/36.6% drop by drop up to 2ml at a time to, shake well, do no allow to over heat.
9. Put in freezer 12 hrs.
10. Filter using buchner funnel, rinse with ice cold acetone.

I washed loads and it refused to go white, how come it is taking so much acetone to wash? I feel I'm using too much to clean. Why is it this colour (please see photo) how can I stop this. I don't know yeild % yet, needs to dry. But I seem to get a lot from this recipe compared to the last I tried.

 

[white7proton]

View attachment vmGnl78Ok4.jpg

 

[hexen]

You need wash him with acetone is dirty

 

[hexen]

And u need use 200ml methyloamine no 160ml

 

[white7proton]

Okay thank you, I will change the amount to 200ml.

I will wash more.

Does everything else look okay in the recipe to you? I feel like I am not doing it correctly.

 

[hexen]

U need heat it 40° 2h on dcm

 

[hexen]

Wash only by water

 

[white7proton]

I'm confused now, can you explain more please, when do I mix with dcm and heat to 40 for 2 hour.

I thought the powder will dissolve if I mix with water?

 

[white7proton]

So when I mix 2b4m with dcm I heat it to 40c for two hours, then after 2 hours I mix with methyloamine slowly and then mix for another 2 hours? Is this right?