I saw a couple things weird about this, though I could be wrong. doesn't this route create a potentially dangerous nitrile byproduct (mmdppn)? also doesn't the reaction between hydroxylamine and helional end up making an amide, not an oxime like shown in the diagram and in the title? I'd be interested in seeing a route that goes through the carboxylic acid (using like dimethyldioxirane and an acid catalyst) as to not generate mmdppn. poison isn't good, avoid poison. instead maybe try: helional -> associated carboxylic acid -> amide -> amine.
@terra-ants1525 yeah the oxime IS the correct product here. You're thinking about the next step. The oxime can be converted to an amide followed by Hoffman decarboxylation to the free amine OR you could use Pd/C and h2 to reduce it directly to the amine
Hi. In the following reaction with Nickel(II) Acetate Tetrahydrate the resulting amide is formed as a solid and extracted by DCM. Any byproducts are left include potential mmdppn. In addition, as I already wrote before here, 1H NMR and GC-MS test haven't detected mmdppn.
@fano72 there's more out there beyond UA-cam. That's all I'm gonna say. This isn't the first channel, they've been making new ones since the old ones got taken down for at least a year now that I've been aware
This reaction is an equilibrium and any unreacted helional is going to be concentrated into the crystals of oxime. You should really do a vacuum filtration and wash with some ice cold ethanol at the very very least. A recryst would be overkill, but any product lost in the washing could be mostly recovered by evaporating but yeah 99% is a bit too high of a yield for this... Love your work btw. Is this new forum going to stay for longer? I got a bit nervous when the other one vanished and quit searching for it
Nice video although why would you make an effort of making an oxime, separate it from the solution and then use it for making amide, if you can go from aldehyd to nitrile to amide in one flask reaction ? Seems a bit outdated.
No it's not new. This guy's been floating around at least a year from what I've seen. Idk what kinda honey pot involves anonymously putting up all the info you could ever want WITHOUT trying to get personal information in exchange
Yeah all the unreacted helional is still present in the "final product" since he didn't filter and wash with cold solvent. It's an equilibrium reaction anyway, and while very high yielding the unreacted starting material is definitely inflating that number considerably
In the method source stated that 1H NMR and GC-MS tests of each synthesis step was carried out. There was no helional or mmdppn as an unreacted and side product respectively. opus.lib.uts.edu.au/bitstream/10453/136093/1/02whole.pdf
@user255 oh yeah same. I get the vibe they're trying to recreate silk road but more DIY based... but if you're gonna build an empire at least come up with your own name!
99% yield is amazing! 👌 love your work! 😊
Let’s gooo! 🎉 👊🍻😊
YYYYES, FINALLY!
Fn crazy I just went from the the gate to check in on vasp and got sucked right into reading about oxides start from the "tom does xy and z " post
I saw a couple things weird about this, though I could be wrong. doesn't this route create a potentially dangerous nitrile byproduct (mmdppn)? also doesn't the reaction between hydroxylamine and helional end up making an amide, not an oxime like shown in the diagram and in the title? I'd be interested in seeing a route that goes through the carboxylic acid (using like dimethyldioxirane and an acid catalyst) as to not generate mmdppn. poison isn't good, avoid poison. instead maybe try: helional -> associated carboxylic acid -> amide -> amine.
an oxime is formed, from which an amide can be obtained as a result of Beckmann rearrangement
@terra-ants1525 yeah the oxime IS the correct product here. You're thinking about the next step. The oxime can be converted to an amide followed by Hoffman decarboxylation to the free amine OR you could use Pd/C and h2 to reduce it directly to the amine
Hi. In the following reaction with Nickel(II) Acetate Tetrahydrate the resulting amide is formed as a solid and extracted by DCM. Any byproducts are left include potential mmdppn. In addition, as I already wrote before here, 1H NMR and GC-MS test haven't detected mmdppn.
@andybbgate oh that's really convenient! Is there any further reading on that nickel transformation step? Ive never heard of that...
@@williamackerson_chemist I've sent the source link in the comment below.
In a similar video, someone said: don't fly too close to the sun 😅
@fano72 there's more out there beyond UA-cam. That's all I'm gonna say. This isn't the first channel, they've been making new ones since the old ones got taken down for at least a year now that I've been aware
This reaction is an equilibrium and any unreacted helional is going to be concentrated into the crystals of oxime. You should really do a vacuum filtration and wash with some ice cold ethanol at the very very least. A recryst would be overkill, but any product lost in the washing could be mostly recovered by evaporating but yeah 99% is a bit too high of a yield for this...
Love your work btw. Is this new forum going to stay for longer? I got a bit nervous when the other one vanished and quit searching for it
Hi, all videos can be found on the website linked in the video. Next video will be there.
Its not. the yields are quantitative, read the literature, they all have the same results.
Nice video although why would you make an effort of making an oxime, separate it from the solution and then use it for making amide, if you can go from aldehyd to nitrile to amide in one flask reaction ? Seems a bit outdated.
There are no clear data conserning this way. Moreover, this way gives good yield.
LOL ... this a complete new style.... id say its a honey pot
No it's not new. This guy's been floating around at least a year from what I've seen. Idk what kinda honey pot involves anonymously putting up all the info you could ever want WITHOUT trying to get personal information in exchange
99% yield ? Questionable.Nice video though.
Yeah all the unreacted helional is still present in the "final product" since he didn't filter and wash with cold solvent. It's an equilibrium reaction anyway, and while very high yielding the unreacted starting material is definitely inflating that number considerably
In the method source stated that 1H NMR and GC-MS tests of each synthesis step was carried out. There was no helional or mmdppn as an unreacted and side product respectively.
opus.lib.uts.edu.au/bitstream/10453/136093/1/02whole.pdf
Breaking Bad might be registered trademark....
I think that's the least of his concerns XD
@@williamackerson_chemist Probably! I just find it odd to use such already taken name.
@user255 oh yeah same. I get the vibe they're trying to recreate silk road but more DIY based... but if you're gonna build an empire at least come up with your own name!
We do not do business with this trademark on UA-cam. We think the name is suitable for the forum.
This is only a forum. The primary site has a different name. Follow the onion QR links to find out more.