I finished the reaction and noticed that when it was done, i had some clear crystal shards already in the bucket, so I drained that off and started reducing the solution. more clear crystal shards, white powdery and pink powdery crystal dust came out of the solution. Anyone know what the shards and white powdery crystals are? maybe just unreacted bisulfite?
/u/earpain · N/A votes · 5th March, 2021 - 14:51 · Link
what's mn(ii)?> Ok I guess I could probably figure you meant Mn(II)SO4 aka Manganese Sulfate. I didnt check Fester's stuff because it's 99% BS, but I found this on wikipedia: "It can also be made by mixing potassium permanganate with sodium bisulfate and hydrogen peroxide." Are you trying to make benzaldehyde from toluene?
/u/nintiesJim · N/A votes · 7th March, 2021 - 12:07 · Link
yes, thats what im trying to do making the manganese sulfate from potassium perm in water with sulfuric acid and sodium bisulfite to do the electrolysis reaction
/u/earpain · N/A votes · 10th March, 2021 - 08:16 · Link
yyes that's a famous reaction. Please, , just please put down Uncle Fester's theoretical ideas he wrote out while spending 6 months in prison for ordering ephedrine. One of the detailed write ups for that reaction can be found on the clearnet, sciencemadness.org. Please respect thhe community, it is not a drug community, but they kind of tolerate it. Search for an old poster cycloknight. He details, with lots of pictures, two ways of making benzaldehyde. The nasty (lol) ellectrolysis with Manganese oxidizer, and one I've done pllenty of times, simple Retro-Aldol condensation cinnamaldehyde ->benzaldehyde. Also there lots of other toluenne->benzaldehyde routes. You know you can do it with just bleach tablets? The kind they put into toilets?> Be careful though! read read read before trying that one.
/u/nintiesJim · N/A votes · 12th March, 2021 - 01:30 · Link
oh yes! ive been to that site before and i know exactly what post you are talking about! I actually plan on testing his one cinnamaldehyde reaction next week with increasing the waters ph and dripping the oil into the reaction
/u/earpain · N/A votes · 8th April, 2021 - 03:24 · Link
Cool! It's probably the best smelling reaction in the histor of drug chemistry. Older literature mentions sodium carbonate, but it turns out just a wee bit of NaOH works better. I never tried dripping the cinnamon oil in, but i'll say this. You can see, and definitely smell the transformation. Cinnamaldehyde smells nice, but so damn strong and aggressive, and it's yellow. As it begins to boil that floating blob of yellow starts breaking off into a definite and distinct blob of clear oil. Both are just slightly more dense than water, but adding any salt at all will push either oill to the top. The real challenge to me was actually fying reliable and cheap sources of either REAL cassia oil or cinnamaldehyde.
/u/nintiesJim · N/A votes · 9th April, 2021 - 07:57 · Link
oh yes, in the past, ive done it with sodium carbonate, refluxed for about 8 hours, then just fractional distilled the reaction flask. i actually plan on trying his NaOH and lecithin method tonight! as for the source of cassia oil and cinnamaldehyde, I actually found a pretty decent source, which they also offer bitter almond oil, at least after you are friendly with them anyways.
/u/earpain · N/A votes · 10th April, 2021 - 05:55 · Link
fractioning column + steam distillation? That must use serious heat or external steam to be effective. Hey i'm working on a new sub, if you want to repost this there, as is or in a different order, i'll respond and hopefully others soon to arrive with gusto! good luck
/u/nintiesJim · N/A votes · 11th April, 2021 - 06:50 · Link
oh, im a pretty low level amateur chemist. i do some stuff because of actually thinking chemistry is cool, while also so I can make some stuff, so there is a good chance that I have been doing it wrong haha, but I wasnt using steam distillation, but I was pulling a strong vacuum, pulling it over at 99-100C and sure! ill do that!
/u/earpain · N/A votes · 12th April, 2021 - 10:14 · Link
with water + the aldehyde?
/u/nintiesJim · N/A votes · 12th April, 2021 - 12:10 · Link
yes. a mixture of the two come over, in the reaction flask remains some of each as well as the unreacted cinnamaldehyde
/u/earpain · N/A votes · 12th April, 2021 - 13:05 · Link
well the chem gods(and i guess laws of physics) say not to do steam distillation under vacuum. They both work via the same principle, they lower the BP of your organic material. Plus no vacuum pump except an aspirator could surive that much water, unless you added maybe a TOWER of dessicant lol.