What do you think about this one?
I've done it but after washing not much was left.
- By 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
↑View previous replies…
- By lamename69
Alright, thanks a lot. Sometimes I wonder where do people get their "this method has the least impurities" agenda. I doubt that every one of them uses lab analysis...
But then I did that method I linked and the product was allegedly awesome. The cooling might not be necessary as you say though.
But then I did that method I linked and the product was allegedly awesome. The cooling might not be necessary as you say though.
- By TheVacuumGuy
Don't know either. They all have "best" methods, but never share it .
I've wasted 20+kg of precursor before i got it right.
Not to say there is still room for improvement though.
I've wasted 20+kg of precursor before i got it right.
Not to say there is still room for improvement though.
- By 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.
- By William D.
You must use dry chemically pure acetone (from the freezer) for washing.
↑View previous replies…
- By lamename69
There's no acetone in this recipe and that's how I know you didn't read it. Acetone is not the only solvent that can be used for washing. Anyway what's most probable is that washing just eliminated BK-4 so I'm essentially asking whether there might be problems with the reaction itself. Thanks.
- By William D.
Acetone is the only solvent that dissolves the product less and dissolves impurities more. We have been working on a better replacement for a long time and there is nothing that works so effectively.
If you do not use acetone, it is better to use crystallization from the aqueous layer. With extraction of impurities with any other suitable solvent.
If you are using real cold synthesis (this thread is about cold synthesis) which can take 1 or 2 days, then it is recommended to use a closed container (under a lid) with the vessel completely filled. This will help to avoid excessive oxidation of the base, which in large quantities can give a brown yellow color and yield losses.
If you do not use acetone, it is better to use crystallization from the aqueous layer. With extraction of impurities with any other suitable solvent.
If you are using real cold synthesis (this thread is about cold synthesis) which can take 1 or 2 days, then it is recommended to use a closed container (under a lid) with the vessel completely filled. This will help to avoid excessive oxidation of the base, which in large quantities can give a brown yellow color and yield losses.
- By lamename69
I didn't figure out that you might have read it and still suggest a replacement for washing. Not my lucky year.
I just thought that there is no way that chloroform would dissolve any of the salt, even if it dissolved less of the impurities. So I was worried whether the synthesis was wrong and your answer didn't manage to touch that, but it happens.
So for crystallization, is there a difference in impurity between crystallizing from a 70% water 30% acetone solution rather than crystallizing from 100% water solution and then washing with dry acetone?
I just thought that there is no way that chloroform would dissolve any of the salt, even if it dissolved less of the impurities. So I was worried whether the synthesis was wrong and your answer didn't manage to touch that, but it happens.
So for crystallization, is there a difference in impurity between crystallizing from a 70% water 30% acetone solution rather than crystallizing from 100% water solution and then washing with dry acetone?