Crude p-TSA Synthesis - [p-Toluenesulfonic Acid #1]

[@j_sum1]

Thanks. I enjoyed this. Looking forward to the cleaned up version. This synth looks to be doable with my skillset and lab. I might have to.give it a go. Subbed. :)

[@SaffronRavenspear]

Cheers mate, I ended up doing one more re-x with ethanol to get a slightly pink, white crystal product... I will get an clean video soon on the next run...

[@good.citizen]

music > chemistry >> thank you beautiful file share

[@SaffronRavenspear]

Thanks mate :D

[@fmdj]

Nice! And beautiful giant glassware lol.

[@EdwardTriesToScience]

cubane for all!

[@SaffronRavenspear]

Cubane for all !!!

[@Ozcanium]

scienceequip coming in clutch with the clevenger apparatus

[@SaffronRavenspear]

You know it brother ..

[@andrews.4780]

Let’s go! Bromine time coming soon.

[@SaffronRavenspear]

[@Exotic_Chem_Lab]

🗿

[@anthenriqe909]

Cool

[@christopherleubner6633]

Distill the toluene, distill the H2SO4, do the reaction, add the tolulene that comes over back in, work up as usual. The black crap comes from napthalene impurities in your tolulene. ❤

[@WackMp4]

😎

[@SciDOCMBC]

I made p-TSA many times before but I never had such a contaminated product.

[@SaffronRavenspear]

Indeed such a crude product, I used way too much sulfuric acid, and made multiple mistakes I shouldn't have.. Will redo this for a pure product very soon and upload a secondary video on this topic .. Wanted to upload this video for anyone interested in this synthesis route, to see errors before doing such reaction to save mistakes for future reference ..

[@christopherleubner6633]

Try distilling your toluene first. The hardware store stuff has all kinds of impurities in it.

[@NuttyGeek]

I am not a certified practicing organic chemist, but I do have several methodological remarks to note. They will ensure higher yealds of the purest product whatever you will be apt to make. Don't take me wrong but my old chemical burns start to itch when I watch your video :) If you think you could feel offended in any way please stop reading and don't proceed any further. In all other cases let us begin: 0:45 This flask is dirtly and wet. It will ruin nine out of ten of you experiments completely or at least drastically impact your yealds. There is a good recepy for cleaning: concentrated h2SO4 with 10-15% H2O2 added later. you don't need much - 15 ml of H2SO4 and 10 ml of H2O2. Beware, it is highly corrosive and agressive stuff. Thoroughly rinse your flask with this solution with a flask closed with stopper and open frequently to avoid preassure buidup. After that dump the cleaning solution to the special bucket filled with solution of neutralizer like baking soda or delute caustic (no more than 10-15%%). Then rinse the flask couple of times with acetone or alcohol of your choice(metanol, etanol, [iso-]propanol). In some cases you may have a need to preceed these final rinses with non polar solvents like petroleum or diethyl ether. Finally when the flask is cristal clean make sure you let it dry completely either in drying oven or on a glassware drier. 0:57 Do not pour reagents from the huge canisters like that. Get a set of appropriate smaller bottles and containers for solid stuff. Firstly it will preserve the purity of the higher volume ingredients and last but not least it will reduce the risk to spill dangerous, expensive or rare chemical. 1:09 Get and use funnels. You've gotta have 4 of them: two glass and two polypropylene/ceramic/PTFE with narrow and wide necks accordingly. 2:33 These gloves do not fit your chemicals, get laboratory high risk latex gloves and make sure to change once you spill the corrosive stuff on. And in most cases try not to reuse once you take them off even if the reaction is not over. 3:37 It is highly recommended that you assemble the whole setup at first, start your water circulation before loading any ingredients. Get multiple-neck (2-4) reaction flask for initial reactants loading and addition funnel for adding stuff as you go with your reaction. Split-neck adapters can be used as well. And by the way all ground glass joints but the receiving flask in cases where applicable must be sealed with silicon grease and locked with clamps. In cases where boiling h2so4 is expected use a drop of h2so4 itself on a male joint and carefully put on the other joint and rotate the joints against each other to ensure they are wetted by the full circle and carefully sealed. It is a preventive action against joints freezing. 11:14 Get a more sutable volume beaker for to get the magnet stirrering rod more efficient. 14:23 This is not a decent vessel for recrystallization. Clean and let it dry completely before use. 14:40 grind the precipitate to fine particles and wash it using appropriate cold solvents that would not dissolve the product but would wash out by-products. Dry it and then go recrystallize. Likes for music, fancy labware and to your successful first stage of the synthesis!~~