How 4mmc cold synthesis is done?

[TheVacuumGuy]

The cold synthesis (some while ago), i do it way different at the moment... more like ( as-hot-as-possible-without-boil) synthesis

 

[animeboro]

How you thing do with dcm and nmp made and then u need use 40min mix ??

 

[TheVacuumGuy]

I don't use both solvents.
There is a post on this forum by @HerrHaber where they do this, as a means of "glue" solvent for the phases. But when you are using a good overhead stirrer you don't have that problem

 

[animeboro]

I know but they get more product in short time

 

[animeboro]

Try use no 300ml dcm but 500ml then u get also more product about ,80% +

 

[animeboro]

your method is one of several cold methods. I started doing it with ethyl acetate in a bottle, I put everything in at once, shake it for 30 minutes and leave it for 1.5 hours until all the 2bromo4methylenopropiophenone is reacted with methylamine and the yield I achieve is the same as yours. but the time spent on the video is appreciated

 

[animeboro]

from what I noticed, the amount of solvent matters, I also use 300ml and my efficiency was lower then

 

[TheVacuumGuy]

This has not so much to do with amount of solvent(s), but whether or not to squeeze some extra from the aqueous layer, which i usually skip. Furthermore on small scale the numbers could be less accurate

 

[Dr. MMX]

btw, its not the best to send direct link wiuth preview on such sites... if youiwanna paste link to youtube make sure it has no preview...

 

[TheVacuumGuy]

Thanks, done.
I actually i dont really care and the vid is "private" bb only takes videos from one of those sites otherwise i hosted it myself.

 

[Dr. MMX]

Its about the youtube which sees where you send the link beacsue of preview
they will probably see that as well without a preview, but for sure a lot of more attention draws when its there

 

[TheVacuumGuy]

Of course they will, with or without preview.

 

[Tovenaar]

Did 50kg on ethylacetate in a hdpe tank with stirrer,

the trick is how to get your temperature under 40 degrees.
2 hours i let the reaction go. Separate, wash, seperate, solvents hcl, filter out product . Then put the remaining liquids in freezer. A few days later take the rest out. Cost me a few hunderd kg bk4 in testing, on top rent workers etc etc….

 

[William D.]

With a large scale, there are problems with ethylacetate hydrolysis. You do the right thing to control the temperature

 

[dnBQByvHb8Zkawbjpx]

Very nice! Would you mind uploading it to BB video library just in case Youtube takes it down later?

At the risk of asking the obvious, in one step you mix the free base with magnesium sulfate - is it implied that you mix it together and filter it immediately through a Buchner funnel, saving the liquid? Or is there any wait time to let the sulfate absorb any remaining water, and can you reuse it after drying (what about other impurities) since 250 g is quite a lot?

 

[TheVacuumGuy]

Well, to be honest, this video is from a year ago, and while it seemed to help somehow (at least in my mind).

Until the moment i found out those were heptahydrate crystals, and did not absorb a single drop . So you can skip that.

This was only to show the "cold" method.

I just finished recording the "now" method, which is so much better that you'd better forget this.

 

[abis777]

It would be nice to share that too. Very nice video anyway

 

[dnBQByvHb8Zkawbjpx]

lmao

please do share your new method, I'd love to see it

 

[lamename69]

What do you think about this one? https://www.reddit.com/r/TheeHive/comments/gngfsa I've done it but after washing not much was left.

 

[William D.]

You must use dry chemically pure acetone (from the freezer) for washing.

 

[Dr. MMX]

there will be difference only in the case if they are there. The most proper way is just to make sure what your using so you will know based on the technique you do what you will face. SOmetimes it can be by "eyes " if something for sure goes bad...
I think H2O is the best solvent for crystalisation, it leads to have avg bigger shards and bigger 1st batch of the yield. In case some discolors are, you can add IPA aclohol to fight it a bit, its usually result of some problems that occured earlier but are shown in the acidification; most likely. DCM is very "weird" solvent and in my opinion its not very good to use it for that reactoin. Usually its "better yield" But rarely it is thing that you would like to have, "washed with acetone, only white left" - dont believe it but consumers don really say it is bad... as looks like

 

[Dr. MMX]

but i would like to prompt my "guess shot" probably partial problem is purity of the final 2b4m as I said in the 1st comment (of your yield and problem of conducting this method) Its the fact it need to be done properly otherwise it cant be saved. Provide us more details. "I did the same" - never happened yet in my life when somebody said that. Its even by the math, you just cant do that, unless its the same line same machine same 1231231 trials before

 

[TheVacuumGuy]

---

Ice cooling bath for reaction seems no good idea. It should proceed as hot as possible. With icebath temp will not go above 20c.
All in all it seems like a lot of extra work compared to recipes here on the forum and videos

 

[lamename69]

Spill the beans then! Hahah. Did you use a recipe from this forum? I've looked through your profile and it seems to me that you have tried a few of them.

 

[Dr. MMX]

@lamename69 I can see you didnt get a reply on your thing. Can you please tell us what would you like to know? Of course I had used, it was the 1st thing on the resaearch on the new genre - its always what you should do. Sadly its addiction, not passion. I gain 12-15h experience everyday
The acetone topic I think it was already explained by William D. I could only add that it really doesnt need to be used for the purification if synthesis is correct, you can do everything " correct" but if you didnt make sure u have "correct" reagents and solvents for it then randomize output goes. I always make. If you inspected my history that much i think you found the (i dont remember now) but over 200g of 300g 2b4m resulting the yield.
Someday addictoin jiust leads to some methhods like this, they are "effective" in the yield, but not in the work. Here usually syntehsis is simple, the guy alraedy had commercial bought as he said so probablyu it was 2 bromo 4 methylopropiophenone, instead of something missed in the ring addictional complications would never happened in the scaled scale becasue it w ould not be worth the effort
maybe.. if 2b4m wopuld be like military would only hunt whole world if somebody has 1 gram... so its so valued to go that path, maybe then

the way the guy did, was very precise he know wyhat he was doing thats why he got that result. You didnt receive it becasue you did a mistake, provide us more details of your syntehsis what went wrong so we can discuss it futher. Without any details we cant tell you anything, we cant even see the question
if i didnt understand that you would like to receive that explaination i am open to tell you, if i can