Mephedrone synthesis (4-MMC) in NMP solvent. Large scale.
Tell me please. Have I correctly calculated the proportions of reagents and liquids in order to obtain 1-1.5 kg of 4-mmc for this synthesis. Thank you!
1) 2-Bromo-4'-methylpropiophenone (cas 1451-82-7) - [1000g]
2) n-Methyl-2-pyrrolidone (NMP; cas 872-50-4) - [3000ml]
3) Methyl amine 40% aq. solution (cas 74-89-5) - [2000ml]
4) Benzene - [6000ml]
5) Acetone - [80000ml]
6) Hydrochloric acid con. aq. solution (HCl 36%) ~ [600ml]
7) Distilled water - [6000ml]
1) 2-Bromo-4'-methylpropiophenone (cas 1451-82-7) - [1000g]
2) n-Methyl-2-pyrrolidone (NMP; cas 872-50-4) - [3000ml]
3) Methyl amine 40% aq. solution (cas 74-89-5) - [2000ml]
4) Benzene - [6000ml]
5) Acetone - [80000ml]
6) Hydrochloric acid con. aq. solution (HCl 36%) ~ [600ml]
7) Distilled water - [6000ml]
After reaching 40 degrees, I start adding m40 in small portions so as not to exceed 55 degrees. I keep the temperature in the range of 50-55 degrees C. With the initial batches of adding m40, the temperature immediately rises when it automatically falls down, I add another portion of m40. After about 15-20 minutes I am only halfway through the planned dose of m40, but when adding subsequent portions, the temperature no longer rises, but only flies strongly down. It looks as if after adding half of m40 and 15-20 minutes have passed since the start of adding it, the reaction has already taken place fully and each subsequent portion of m40 (only half has been added) no longer raise the temperature but only cools the solution strongly. What am I doing wrong? In the end, the performance reaches 20%, and the final product pinches the eyes and bites the nose.
- By G.Patton
Hello. Have you washed your reaction mixture by water after reaction? (step 4)
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Yes, equal to the volume of water twice and once 10% sodium bicarbonate solution. I am surprised by the very low efficiency where I get about 53-55% on the crystal. It is also strange that when I add half of the m40, at the second half the reaction is no longer exothermic, and the temperature during addition only drops down.
Acidification always leads to PH around 6. When you write about the refrigerator, you mean putting the neutralised freebase in the fridge to make the whole product fall out? Do you think so much product could have been dissolved? Is it normal that after adding half of the m40, the temperature stops rising on its own and the whole thing cools down? Thank you for your help
- By G.Patton
>>>When you write about the refrigerator, you mean putting the neutralised freebase in the fridge to make the whole product fall out?
yes, exactly
>>>Do you think so much product could have been dissolved?
I can't answer
>>>Is it normal that after adding half of the m40, the temperature stops rising on its own and the whole thing cools down?
Yes, it is okay. If you want to check conversion of reagents to 4-MMC, you can use TLC (look at Lab FAQ).
yes, exactly
>>>Do you think so much product could have been dissolved?
I can't answer
>>>Is it normal that after adding half of the m40, the temperature stops rising on its own and the whole thing cools down?
Yes, it is okay. If you want to check conversion of reagents to 4-MMC, you can use TLC (look at Lab FAQ).
I have a question, the one who recorded these videos probably saw what he was doing but what was written is not true. in the video you can't see that two solvents were used for cooking and only one was then washed with freebase with water and ethylene acetate and that's it, so where does anyone see benzene??
The resulting 2-bromo-4-methylpropiophenone in benzene is poured back into the clean flask and provides 200 ml of 40% methylamine (aqueous). Connect the reflux condenser, flask and thermometer (preferably) to the flask. Combined stirring and slightly warming the mixture (30-40 ºC). When the basal temperature, add as much as 300-400 ml (just use more). N-methylpyrrolidone from the dropping funnel (trickle), making sure the temperature does not exceed 60ºC. When adding N-methylpyrrolidone exothermic reaction, temperature can help. If the hands are too straight, it is a sign of overheating, it is recommended to slow down the mixing a bit to keep the temperature in the upper right corner). Once all the N-methylpyrrolidone has been poured in, let it mix for another 15 minutes. The entire reaction takes 15-25 minutes.
When we have pure powder bk4 then we use only NMP and methyloamine to cooking only...
When we have pure powder bk4 then we use only NMP and methyloamine to cooking only...
About the video, someone would know to say:
1) Which mechanical stirrer is used? Top mechanical stirrers often look like a metal rod rather than PTFE.
2) How is the emptying done in the system? through which RBF tubing?
See that the system has negative pressure and he uses this to feed the RBF with reagent liquids through a hose.
Thanks!
1) Which mechanical stirrer is used? Top mechanical stirrers often look like a metal rod rather than PTFE.
2) How is the emptying done in the system? through which RBF tubing?
See that the system has negative pressure and he uses this to feed the RBF with reagent liquids through a hose.
Thanks!
- By G.Patton
Hi, not so matter. I would recommend you to use PTFE if it possible.
Use vacuum pump and silicone hose. What is problem and what don't you understand?
Use vacuum pump and silicone hose. What is problem and what don't you understand?
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- By malignoalfa
They use five-necked RBF.
1) mechanical stirrer
2) thermometer
3) condenser
4) addition funnel
5) Valve with supply hose
My question is: how is the vacuum made in this setup?
thank's for your time
1) mechanical stirrer
2) thermometer
3) condenser
4) addition funnel
5) Valve with supply hose
My question is: how is the vacuum made in this setup?
thank's for your time
- By G.Patton
You have to use vacuum pump. You can utilize aquarium pump in order to pump liquids. Also, read Laboratory FAQ section => Providing and application of vacuum in a laboratory
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