PoorMansChemist profile
PoorMansChemist
PoorMansChemist
Chemistry experiments and demonstrations with a focus on making unusual and not often seen compounds.
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PoorMansChemist

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PoorMansChemist
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Holy sheep shit, ladies and gentlemen, I think I just figured out a way to deal with the copious amounts of HCN gas needed to make pure TlCN solution. TlCN can be precipitated from a solution of thallous nitrate by addition of aqueous potassium cyanide but the yield sucks. TlCN is NOT all that insoluble despite the way the literature reads. 100 grams of water dissolves 8.67 grams at 0°C, 15.17 grams at 14°C, and 29.57 grams at 31°C. The other way to make TlCN is to bubble HCN through a solution of TlOH. This reaction has to be done way back away from the house but up until now I've had serious concerns about going near it to adjust anything and especially breaking down the apparatus. HCN is lighter than air but not by a whole lot so I would imagine that it rises slowly. That gives me pause. But apparently this whole problem can be solved quite easily by simply breathing through a very long garden hose whose far end is way way away on the other side of the property. So long as I breathe in through my mouth and out through my nose I think it will work. I should stress this is only to buy me enough time to make whatever adjustment needs to be made or to open the apparatus to degas at the end. Sure in principle this should work perfectly. In practice having tried something similar already in the past I know its not quite that easy. But I think I can pull it off. Obviously don't try this at home kids. 
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PoorMansChemist
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Seriously Atomistry?
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PoorMansChemist
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Damn it. I am out of both aqueous ammonia and nitric acid. I can make up a batch on one tonight and a batch of the other tomorrow. But it's supposed to piss rain for the next two days. I was going to do diamminedichloropalladium(II). I still might. I would just need to bubble some of the NH3 from the ammonia generator through the suspension of PdCl2. It makes a dark tan precipitate in water. Atomistry describes it as a "flesh colored precipitate". While it is indeed what anyone today would call a flesh tone I'm not sure if someone in Europe a century ago (which is when and where I think the source material comes from) would call it "flesh colored". I'm not saying it's "muh systemic racism" or anything like that. I'm just saying that people looked at things differently a century ago and I'm trying to put myself in their heads. Anyways we could go a different way with this and make up palladous sulfide PdS, filter it, dry it, and then fuse it with 12 parts KOH and 12 parts S powder to make potassium thiopalladite K2Pd3S4. I have more than enough fuel for an H2S generator. Either way I have to set up a gas generator.  
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PoorMansChemist
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The next organic video will be out within the next week. I'd also like to do a short video on the oxythallation reaction since it's such a neat trick. The next prep video will be the diammoniate of palladium(II) chloride PdCl2(NH3)2. After that I want to do a prep of palladous sulfide and from that make potassium thiopalladite K2Pd3S4 which is supposed to be a violet-blue turning gray when it dries. That sounds pretty neat. Not sure what we will do with the diammoniate. Maybe use it to make bis(acetonitrile) palladium(II) chloride if possible. It would finally give me something useful to do with all this ACN. 

This is how I will make the diammoniate. This comes from the Atomistry page for palladium dichloride. "When palladium dichloride is dissolved in water, and ammonia added in sufficient excess to dissolve the flesh-coloured precipitate, the diammoniate, PdCl2.2NH3, may be obtained as a precipitate by diluting with a large volume of water and acidulating with hydrochloric acid. It may be dried at 110° to 120° C., and has been used for the determination of the atomic weight of palladium. Density 2.5."
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PoorMansChemist
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I finally figured out what George Trepal was doing (or at least I'm pretty sure I've figured it out). We know from his criminal history that he had some kind of thallium compound left over from his days running a meth ring. So somehow this dude was using thallium in the production of meth. I had never heard of such a thing before. But as it turns out running an oxythallation reaction using thallium(III) nitrate on alpha-methylstyrene produces phenylacetone in 81% yield. That has to be what he was doing. I have to say it's a clever precursor to use and it's a fascinating way to use it although the best dude could have hoped for was the prep of a racemate by this route. Which is kind of lame. This is before the days of PE being regulated. Dude could have been making enantiomerically pure product without having to work with thallium quite easily. Oxidation with bis(pyridine)silver(I) permanganate followed by a Clemmensen reduction would have done the trick I think and it probably would have attracted less attention. I'm really having a hard time accepting that this guy was in MENSA because he was pretty damn stupid.
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