Did you consider using a short path distillation setup for the phenol distillation? That's how I normally do it and with the distillation path being so short, you don't have to worry much about it solidifying in the condenser and clogging it.
Usually phenol and hydroquinone (and other phenols), are cheaper than salicylic acid, genistic acid etc. Industrial production of salicylic acid and its derivatives, like aspirin, and parabenic acid, are usually carried out from the alkaline phenoxide and CO2, under pressure. Initially the orto carboxylate is formed, but over time, the para carboxylate is favoured thermodynamically. (In the "Kolbe-Smidt reaction"). I haven't tried decarboxylation of the parabenic acid, but I guess it's just slightly more stable than the salicylic acid.
I'm glad you did this. When I was doing it I went with refluxing the acid using an air condenser, medium heating and more time. Basically slow cooking until it was all decomposed. It took few hours. Blasting it with high temperature of the flask bottom promotes localized reactions that lead to tar and, while I can't be sure about this, I always fear there could be biphenols. After refluxing, I did two distillations with air condenser. Residue was negligible and yellowish. Use as small storage bottle as possible to avoid oxygen, or purge air out with argon/nitrogen. It will prevent phenol going red and damp. Very useful chemical for microscopy and fixating tissues.
I was thinking about preparing catechol from salicylic acid by esterification (to e.g. methylsalicylic acid) followed by Bouveault-Blanc reduction (sodium in ethanol). Another possibility would be decarboxylation to phenol (as in your video), formylation to salicylaldehyde and finally reducing the aldehyde group.
Very nice! What supplier did you get your salicylic acid from? I'd like to make a good batch of phenol soon but I can't bear to do yet another Asprin extraction lol.
Phenol as a solid, when used in reactions isn't too scary. It is toxic, but it's not too sketchy. Distilling phenol is very scary tho. It requires pretty high temperatures, the distillate can solidify in the apparatus, and well, gasseous phenol is WAY scarier than normally. It's a lot better to buy phenol if you can, than to make it, but well, not everyone can buy it.
i remember one guy added in a mixture of copper salts for the decarboxylation of salicylic acid, supposedly it catalysed it somehow. might be worth a try if anyone plans on doing this i suppose non-oxidizing copper salts like copper acetate chloride and sulfate would work phenol is very toxic, but if you dilute it up with a lot of oil its a very efficient disinfectant, as in to be used for infections rather than cleaning surfaces
The internet contains all sorts of information..... www.google.com/search?q=phenol+to+aniline&source=lmns&hl=de&sa=X&ved=2ahUKEwi97Y2nlbT4AhWUVvEDHeV_Ah0Q_AUoAHoECAEQAA
Did you consider using a short path distillation setup for the phenol distillation? That's how I normally do it and with the distillation path being so short, you don't have to worry much about it solidifying in the condenser and clogging it.
Yeah I’d have done that but there’s no short path distillation bridge in my possession yet
@@THYZOID oh okay. Yeah they are extremely useful for things like that and that was the main reason why I got one years ago. Definitely worth getting!
Usually phenol and hydroquinone (and other phenols), are cheaper than salicylic acid, genistic acid etc. Industrial production of salicylic acid and its derivatives, like aspirin, and parabenic acid, are usually carried out from the alkaline phenoxide and CO2, under pressure. Initially the orto carboxylate is formed, but over time, the para carboxylate is favoured thermodynamically. (In the "Kolbe-Smidt reaction"). I haven't tried decarboxylation of the parabenic acid, but I guess it's just slightly more stable than the salicylic acid.
I'm glad you did this. When I was doing it I went with refluxing the acid using an air condenser, medium heating and more time. Basically slow cooking until it was all decomposed. It took few hours. Blasting it with high temperature of the flask bottom promotes localized reactions that lead to tar and, while I can't be sure about this, I always fear there could be biphenols. After refluxing, I did two distillations with air condenser. Residue was negligible and yellowish. Use as small storage bottle as possible to avoid oxygen, or purge air out with argon/nitrogen. It will prevent phenol going red and damp. Very useful chemical for microscopy and fixating tissues.
I was thinking about preparing catechol from salicylic acid by esterification (to e.g. methylsalicylic acid) followed by Bouveault-Blanc reduction (sodium in ethanol). Another possibility would be decarboxylation to phenol (as in your video), formylation to salicylaldehyde and finally reducing the aldehyde group.
How convenient, was planning this synthesis! Awesome work!
Very nice! What supplier did you get your salicylic acid from? I'd like to make a good batch of phenol soon but I can't bear to do yet another Asprin extraction lol.
Maybe from cosmetic ingredients suppliers, or a lab chemical supplier (if available).
I got my salicylic acid fr a German chemical supplier called S3 chemicals
It can easily be found on eBay or Amazon.
@@BackYardScience2000 I know, but I'm always looking for new suppliers to see what's more affordable and to browse their selection of chems
0:35, you know what els is a fluffy white powder
Magic 😂
I'm doing this today to make an azo dye.
Phenol as a solid, when used in reactions isn't too scary. It is toxic, but it's not too sketchy. Distilling phenol is very scary tho. It requires pretty high temperatures, the distillate can solidify in the apparatus, and well, gasseous phenol is WAY scarier than normally. It's a lot better to buy phenol if you can, than to make it, but well, not everyone can buy it.
German Chemists are really the best. I’ll have to use this technique myself in the lab next time I need some Phenol!
An organic chem professor on mine once said "Chemistry is German".
* of mine
Can you make flaks put of phenol and not a solid mass?
Almost missed this one D:
Why you not use decarboxylation reaction using naoh/cao.
Why use this route if decarboxylation without any additional reagents works even better?
Can you just cook sodium salicylate and distill off the phenol, leaving sodium carbonate? Or is that a dumb thing that wouldn't work.
You’d have to research it. I don’t know.
i remember one guy added in a mixture of copper salts for the decarboxylation of salicylic acid, supposedly it catalysed it somehow. might be worth a try if anyone plans on doing this
i suppose non-oxidizing copper salts like copper acetate chloride and sulfate would work
phenol is very toxic, but if you dilute it up with a lot of oil its a very efficient disinfectant, as in to be used for infections rather than cleaning surfaces
Copper acetate decomposes at moderate temperatures. I wouldn’t recommend it because of contamination.
@@THYZOID hm yes, copper oxide can work as an oxidizer and that might be what copper acetate eventually decomposes into
I recommend putting some clear plastic tape over your labels to make them more waterproof
Have you looked how the label was glued to the bottle?
@@THYZOID My bad I did not see it clearly.
Could you have purified the phenol by an acid base extraction instead of distillation?
Maybe but distillation should be the easiest method
now how do I turn phenol into aniline
The internet contains all sorts of information.....
www.google.com/search?q=phenol+to+aniline&source=lmns&hl=de&sa=X&ved=2ahUKEwi97Y2nlbT4AhWUVvEDHeV_Ah0Q_AUoAHoECAEQAA
Hi, I just wanted to say, I love your Videos
I appreciate it!
From where is this stirring mantle, mate?
Got it at a lab shop nearby
@@THYZOID thanks, it is at good price and quality also!
+
THYZOID LABORATORIES Phenol has just one annoying property: it oxidizes in air quite easily into hydroquinone.
What thermometer are you using?
ua-cam.com/video/YBhDj5ZXlg0/v-deo.html
Ah yes, the salicylic acid decarboxylation, right of passage for chem youtubers lol
Can you try decarboxylation of tryptophan?
That one is probably illegal here. Any other recommendations?
@@THYZOID I figured 🙂 Maybe nitrostyrene from scratch, that would be cool. You are missing some nitro chemistry
👃🩹 the classic smell of plastic bandages at least for Band-Aids in the US.
I am going to be doing this one soon and its good to know a few tips ahead of time. Great video if I could subscribe again I would!
Stay safe phenols vapors are not healthy. I wore a gas mask because a lot of vapors were released.
Definitely! I have one its a half face respirator but really should invest in a better one kind of like what you've shown to better protect myself.
Next video catecol from phenol 🙏
The phenol is already planned to be used up for Trifhlorophenol completely. Maybe in the future
Now make Penolphtalein out of it 😉top work 😁keep it up pal 😎👍
and? so what now???
witzig, ich hab vor nicht mal 30 min das video von nile red dazu gesehen