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This is such a breeze compared to the Br2 route in DCM/Toluene ❤️

2.5 hour in 60c toluene ? And at which point is NMP added (as shown in complete video tutorial in benzene)?

I think your problem lies in the previous step (eg. Filtering precipitate. It may be white, but off-white often also appears white). For crystallization you could use 2 beakers. In 1 you add water and boil it. In 2 you add dry powder (and/or) a stirbar. Then you slowly pour the some water from 1...

I wouldn't recommend anything yet, since i'm talking about specifically the colorization issue. Using different solvents pose other problems further up, But in this case it is ethyl acetate

You will often get these comments or questions: Unreacted methylamine ? Unreacted bromoketone ? Acid added too fast ? Temps too high ? Bad XYZ? The answer to above questions is : probably not. The colorations are caused by acidification in acetone. How and why is yet to be determined...

strange, i've monitored temperature closely a couple of batches (every 5 minutes), and it shows that temperature will decrease after ~55 min while still have amine remaining to add. when adding this remainder all at once, the temperature does nothing, it will keep decreasing.. this would...

KING! Tried a small 25g batch, acidified from the bottle by eyeball, so of course too large portion instead of dropwise, but somehow magically it went straight 5.5, so was done in 1 second. (method used as discussed in this thread, NMP, but replaced benzene for DCM).

directly going to try this acidifcation using ethyl acetate. getting sick of playing poker where 2 batches are geenred and 1 perfect white at random.

single ticket to garbage can

wait until you smell 2b4m. i'd rather swim in benzene

Man, throw it away

Please enlighten me. Why would one add more acid when ph target reached?

Just do even amount of 10% sodium bicarbonate water solution (baking powder). Then wash with even amounts of water. Shake, repeat. Until the freebase is clear not cloudy and/or water layer is clear so you'd drink it. That clean .

Aren't those linked? I mean too much unreacted bk4 would also mean too much unreacted amine and vice versa.

Hmm. I might just go about concentrating the 30% stuff by dripping it into sulfuric acid and lead the gas to an inverted funnel setup in a beaker containing highly chilled hcl 30%, setup in an icebath. The problem is that it is a lot of work and messy (esp. cleaning up) for rather small volumes

Sharp! :) luckily these don't require an end-user-statement. Let me rephrase the question: What i'm looking for is a purpose/use-case which would justify 37% HCl over 30% HCl , that is: what procedure really needs 37% HCl, where 30% would not suffice, or would cause quality issues.

Hi all, Could anyone provide me with a "use case" for 37% HCl? i searched for several days and came to the conclusion there is none, really. However, it is asked when ordering this.... needless to say, disclosing the real intentention would not be a good idea ;)

see @w2x3f5 's answer above. or mine, another one above. And if - As a beginner in chemistry, don't expect it to succeed instantly... prepare to waste multiple kg of bromoketone on failures before you understand what is going on, and good things happen. Oh , almost forgot. Don't let color fool...

And strange it might sound, over acidifying sometimes ends up very well. A week ago, the valve of the dropping funnel was loose, ph 1.5, yet a highest yield and beautiful white product.

And don't forget to freeze it afterwards to become thicker.