If I didn't crystallize at least 3 times, I couldn't stop :) If you want purity, you have to make an effort. This is a great post, I follow your work with pleasure. Are you an academic?
Dissolve a bit of lithium metal in 100ml of methanol. You'll end up with a methanolic solution of lithium methoxide which burns with a beautiful crimson red flame. The contrast between burning trimethyl borate and lithium methoxide is simply gorgeous.
Very nice. Did you add a stabilizer or were you using it quickly? Something like hydroquinone or tert-butylcatechol? Also did you ever check the concentration? I think this method is a good solution for me I am just curious how it worked out for you in the end?
I didn’t add any stabilizer, just stored the aniline in an amber bottle away from light, over time the aniline will darken regardless. I didn’t do a titration to determine the exact concentration/purity but it should be quite pure after distillation. Many other people have replicated my procedure (there are some other videos posted about this reaction on RU-vid now) and they have had good results as well!
What do you mean due to the loss of vacuum in the system? Dont you keep the vacuum pump running during the distillation? Or do you pull the vacuum, close the system then run the heat to distill product? I always thought they say to keep the vacuum pump running during the whole process and have a vacuum constantly pulling on the atmosphere inside the system? Im confused lol
Do you by any chance know if you can make acetic anhydride by reacting succinic anhydride with acetic acid? It's something i have been asking myself for quite some time now, i just don't have the time to experiment myself lately.
I'm confused why you called the step of mixing with HCl "quenching". I see how that's where you're moving from one phase to another in the procedure, but the real quench IMO was when you turned the hot plate off, since this was a pyrolysis. The other way this could be quenched was if you were deactivating the reagents with HCl, but the catalyst would be unaffected.
Congratulations to you for reaching 5k! Well done, I was happy with your results and the analysis was well documented too. I do wonder if there would be interest in some glassware cleaning ASMR? ^^
With the large difference in Rf between the desired product and the unknown non-polar impurity, it might make sense to run a column long enough to discard that first fraction. It's a lot of material to process though at this scale.
Hello, could you give a video tutorial on the synthesis of triethylene glycol ditmethacrylate (CAS 109-16-0) and DIURETHANE DIMETHACRYLATE, MIXTURE OF ISOMERS (CAS 72869-86-4)
One use I found was as a starting material for the total synthesis of chlorophyll A, which I'm sure involves a tremendous amount of work as the intermediate chlorin-e6 trimethyl ester took 46 separate steps to produce according to the summary of the paper.
Did this synth a few years back during an internship. I remember this compound smelling really bad. The PhD student said it smelled like horse piss to him
