Well, I'm working from Post 251119 (https://www.thevespiary.org/talk/index.php?topic=11878.msg25111900#msg25111900)
(Bandil: "Nitroethane ala Antoncho succes", Novel Discourse), which was of course inspired by Post 233762 (missing)
(Antoncho: "Kitchen nitroalkane success!", Chemistry Discourse).
I started w/ same materials and quantities, only after dripping the EtOH into the H2SO4 initially I let it sit, covered, overnight because I had to get some sleep. Then tonite I heated it back up to <100C (thermometer broke last week, new one is on order) but warmer than body temp (hot to touch water bath but not burning my gloved finger), so maybe 40C. I measured out 60g's Na2SO4 and poured a bit at a time in, and observed it to bubble, then dissolve slowly each time. Then I got bold (read that, "stupid") and poured in a bit more, say 10-15g (previous portions had been 3-4g) and it foamed up to way above the liquid line and locked up solid... my little 1" stirbar in 500ml RBF is completely overwhelmed.
I've just come from trying to figure out how to loosen this stuff up, it's not WET anymore, it's the consistency of pizza dough and even replacing the 1" stirbar with a 3" hasn't helped noticeably... so I grabbed my thermometer (did I mention it broke?) and have been shoving my 3" around, hoping to loosen things up/encourage absorbtion/fix the mess I have made while having followed (I thought) word for word what has worked in two different bees' kitchens.
I don't see a graphic for a sigh, so:
Suggestions?
Swim has to assume that swim chose a flask that was too small for the reactants to react.
Swim added ~160mls Ethanol (the same 93% denatured as used in Post 251119 (https://www.thevespiary.org/talk/index.php?topic=11878.msg25111900#msg25111900)
(Bandil: "Nitroethane ala Antoncho succes", Novel Discourse)), and it just *sat* there on top, this stuff is horrible. So swim capped it and shook it, and finally got it to be a little thinner. Swim still doesn't think he managed to get to where his 1" stirbar was moving at all, but swim was almost out of flask and certainly out of patience.
Swim is turning it all off for the night. The references both have FILTERING after cooling at this point... hahaha. I'm beginning to wonder if my "Glauber's salt" isn't Na2SO4 but something completely different, and I've just wasted a night. Either that or there is a level of stirring to be had that's beyond my current experience. But whatever these guys did that I didn't, the pasty white stuff I have filling my 500ml RBF is a terrible mess and a real disappointment.
Thx for the suggestion, tho, Rhodium.
What "cold method" have you had problems with? I have heard no complaints about the cold method using Ethylenediamine Diacetate (https://www.thevespiary.org/rhodium/Rhodium/chemistry/edda.html)
(https://www.thevespiary.org/rhodium/Rhodium/chemistry/edda.html)
If you do end up with an oil when making a nitroalkene, pour it into cold water and extract with ether until the aqueous layer becomes colorless, wash the pooled etheral extracts with brine and distill the ether for re-use on a 50°C water-bath (to not overheat the nitroalkene). The nitroalkene should now be crystalline. Dissolve it in a minimum amount of boiling iPrOH and let cool slowly, first at room temp, followed by the fridge. Filter and wash with a small amount of ice-cold iPrOH. The filtrate can be chilled in the freezer to precipitate a few further percent of impure nitroalkene, but this is usually not worth the effort.