Synthesis of 4MMC in benzene

[Chemix-Express]

Hello, I currently produce a very high quality 4MMC in benzene. No less in my country its purchase in larger quantities is quite cumbersome.

I have heard from some sources that it can be interchanged 1:1 with Toulen. In benzene I run the reaction for 3h at 60 degrees. For Toulen will it be identical?

The amount of solvent used in the reaction will also be the same?

Thank you for your help

 

[subzero013]

the reaction time and temperature regime when using toluene are the same as when using benzene. You can try ortho xylene, the time/temperature is the same. it is less toxic than benzene, causing less suspicion.

 

[Chemix-Express]

Full respect for your help. I will keep trying.

After many attempts and hundreds of g converted, I finally arrived at a high yield with maximum powder purity just after acidification, even before rinsing with acetone.

Whereas previously I needed more than 15L of acetone for 1kg of 4MMC gunpowder to make the filtrate transparent, now 4-5L is enough. The result is immediately apparent when crystallising such pure gunpowder.

Power to you and thanks for the valuable tips

 

[subzero013]

One respected chemist wrote that on benzene / toluene / ortho-xylene at 60 degrees, the reaction is held for 2.5 hours, the time to reach 60 degrees is considered 50%. If the solution is heated to the desired temperature in 20 minutes, it is counted as 10 minutes and the reaction is kept at 60 degrees for another 2 hours and 20 minutes. at a temperature of 60 degrees, overheating is very dangerous, it seems like dirt and isomephedrone begin to crawl out very quickly in a few minutes. if the synthesis is carried out at 50 degrees, then the reaction takes 4 hours, perhaps this option will suit you even more. I almost always worked with dichloromethane, but with it the synthesis is not as smooth as with benzene / toluene / ortho xylene.

 

[Chemix-Express]

The more purity and efficiency I managed to achieve, the more confident I became that I knew all about synthesis in Benzene....

A stupid man is born and a stupid man will die

Btw.
Last time it took 3h and 10min from reaching 60 degrees to turning off the heating and proceeding to flush the free principle.

There wasn't a lot of contamination at first glance, but the familiar smell of dimmer in the dry powder 4mmc kept me guessing.

Now I know why, I counted the time from reaching 60 degrees.



For clarity. I divide the time that elapses between pouring the m40 and heating the whole thing to 60 degrees in half and include it in the reaction time.

The entire response is expected to take 2:30h including the time divided in half from the addition of m40 to reaching 60 degrees?

Looking at the time-temperature relationship tables in a given solvent, it appears that the maximum yield is for a 3h reaction at 60 degrees and this is what I was guided by.

I will use your advice at the earliest opportunity hoping to raise the quality further upwards.

How can I repay you for your help?

 

[subzero013]

I remember this table), if I am not mistaken, the lynx wrote that the proportions were used here - 1 mol of bromketon per 1 liter of solvent. In the prescription where the time was indicated for 2.5 hours there was a proportion - 1 mol per 375 ml of solvent (benzene/toluene/ortho xylol. Perhaps this is somehow influenced, but even if you rely on the table, the difference between 2 and 3 hours is scanty, only now appears A little isomefhedron. It’s easier to wash the residues of BC than isomefedron, you can simply acidify by adding water and hydrochloric acid, then evaporate the water completely or to the desired volume and already release the meferon with the addition of acetone and cooling in the freezer. Everything you have a rotary evaporator, then simply Drive the water and that's it. The output is super small crystals, but they are easy to wash and you will not pull many substances from a layer of benzene/toluene, no resins, light filtration and washing, there are a lot of advantages.

 

[subzero013]

I also read that it is impossible to brominate in Orto Xille, as it reacts with bromistic acid, so either bromine in dichlormethan and drive it away, or through hydrogen acid and already crystalline bromachon (completely washed from acid and bromine) dissolve In Ortoxilol and work with him.

 

[Serega]

Bro, you're right. but!!! bromination can be done in dichloroethane (boiling point >75°C), but not in dichloromethane (boiling point 38.5°C).

 

[subzero013]

why can bromination in dichloromethane not be carried out? what does his boiling point have to do with it?

 

[Serega]

depending on the method of bromination. for bromination with bromine DCM is suitable. and for bromination with HBr + perhydrol is not suitable, as the reaction is too exothermic, and DCM foams strongly and boils away

 

[subzero013]

I kind of pointed out that in dhm with bromine, maybe the translator fails, I will double-check now. with Hbr and peroxide, the same solvent is not needed.

 

[subzero013]

by the way, maybe you know. How long can you store 4mpf at room temperature and frozen (in the refrigerator)?

 

[Chemix-Express]

I don't know if this will help you, but 4mmc in powder or glass after a few weeks at room temperature completely unchanged. Power, aroma unchanged.

 

[Chemix-Express]

Hi. How many litres of solvent in the form of Benzene / Toluene is it best to use for 1kg of BK4? The reaction would be carried out at 60 degrees. How long should the reaction take at 60 degrees, 2.5 or 3h? Should the time needed to heat the mixture to 60 degrees be counted as half or not included in the reaction? After the animation stage, what is the best way to rinse out the free base? Water alone several times? Sodium bicarbonate? Sodium hydroxide? After cleaning I intend to pour in an equal volume of ethyl acetate and dropwise add hcl 35-37% in water. At the end of the acidification stage, for how long is it best to put the whole thing in the fridge/freezer? Can I then use dry ice to speed up the process?

 

[Chemix-Express]

Anyone have anything?

 

[Chemix-Express]

I would forget. I always acidify to pH 7, is there any point in going lower and if so to how many?

 

[StarWars]

Im made with ethyl acetate and im shake 30,min only and finish product is perfect
Ph 6 to 5.5.
7 is to much

 

[Chemix-Express]

Can you describe how you manage to do this and with what efficiency? Even on pw if it is a problem so that a wider audience can see it. Interesting topic let me tell you

 

[StarWars]

I was send u message on PW