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Questions for Lestat: Lestat's Lab

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renaeden:
I especially like that last picture, they're cool (and tiny!).

Lestat:
TY Ren.

And they don't need to be large, in fact it's more advantageous that they aren't, that way, the same test can be carried out with just a few milligrams of material, that if a standard test tube (which would receive more uneven heating, unless perhaps were it to be done by immersing a tube within a tube, an inner, cold oil bath placed in a hot one, with the test tube holding the sample inside that, nested like russian dolls) were used, instead, would require hundreds of mg at least. Which isn't in the least desirable if the material is heat-sensitive, or decomposes upon melting, and all the more so if it's something that requires expensive precursors and reagents to create, and/or if it's something particularly biologically potent, that one either wouldn't want around in larger quantities due to the danger of accidentally poisoning oneself by contact with traces or otherwise coming under the influence of it in an un-intended way (just think about Albert Hoffman and his fortuitous discovery of LSD, that famous bicycle ride home...he was a meticulous synthetic chemist, working on ergot alkaloids, in the hope of discovering derivatives with oxytocic (uterine-contraction-inducing/cervix-dilating effects) properties. It just so happened that one of them, LSD-25, the 25th in a series of creations, was extraordinarily potent, and that even with his great care; he came into contact with a tiny trace, perhaps a speck of dust loosed into the atmosphere during weighing, or putting it into a bottle, maybe taking a glove off with a tiny amount on it, absorbed through his skin or traces finding their way to fingers which contacted something he ate or drank after, who knows, he probably never did, that was enough to cause a moderate acid trip, the first one in history, that was subtle, due to the tiny amount he absorbed even despite due diligence, but he noticed the effects on his perceptions during the famous bike ride back home from work, and it gave him some sort of intuition about it, to revisit i and examine the otherwise unpromising compound in further detail)

That turned out benign, and for the betterment of mankind, but had he been the discoverer of one of the ultrapotent etorphine or fentanyl pattern opioids, what would be a bare threshold dose of  LSD, say 25-30 micrograms would have killed him many times over, fentanyl itself being about 100 times the potency of morphine, and the most potent of the series, one of the analogs of ohmefentanyl, the most potent of it's stereoisomers has a derivative which is around 30,000 times as potent by weight. Fentanyl itself is already capable of killing somebody by absorption of a minute particle  far too tiny to see save perhaps with a very good microscope in the right situation, set up to look right at it, thats a 100-fold increase in potency compared to morphine (the baseline standard by which all opioids of the Mu-opioid receptor ligand type are measured), and compared to that compound, a fluorinated analog of beta-hydroxy-3-methylfentanyl, the most potent of it's stereoisomers, it's still like comparing a nettle sting to an armor-piercing/explosive/incendiary special purpose .50 caliber BMG heavy sniper rifle round. It wouldn't be enough to just have killed him, but probably have taken anyone that did an autopsy on him with him to the grave, hell, possibly enough to knock off the people who autopsied the pathologists, and anyone stupid enough to dissect them too, just from skin contact with a stray droplet of blood.

Although I personally, have a great dislike for fentanyl producers and producers of it's relatives and similar ultrapotent opioids outside of actual highly controlled neuropharmacology research, it's irresponsible, stupid and panders to the nastiest, greediest elements connected to clandestine chemistry, gives people like me a bad name by association. And I won't work for people who ask that kind of job done by me, doesn't matter the pay, I just won't do it. Not only because I personally, want to keep on living (weight for weight, unmodified fentanyl still requires a smaller dose, by far, than VX nerve agent to kill someone non tolerant to opioids, dermal exposure or inhalational exposure to VX requires about 10mg for a 50% kill chance, of a 70kg adult male human, the lowest dose fentanyl patches, IIRC, deliver 25 micrograms PER HOUR (that said, if one of the two was going to be what eventually means my exiting this world on a permanent basis, I know which it'd be if I had a say in the matter :autism:, and with a tolerance, admittedly, I have tried those patches and I found them to be fucking awful at that dose, GP tried me on the patches once, and I didn't even last a full day. Worked out in the end for me well enough, as I had picked up the oxycontin 80 script I was using at the time for pain control on the monday of that week, had a consultation with the GP the next day, where she suggested I try fentanyl patches, I agreed, only to find out wearing one wasn't even enough to prevent me withdrawing, and went back the next day to ask that I be changed back to how things were. Didn't expect to have anything actually different done that day, just go back next week, as I'd already picked the oxy up on monday, but the wednesday I went in to complain because I was both withdrawing if using as prescribed (ended up having to extract and shoot the contents of the patches to get through that day, although could have used the oxy.  And found out that I just hate fentanyl full stop, it's bland, sod all rush on IV, cold, clinical, boring and generally....just...meh...ick....) but she said sure, I'll switch you back, ended up printing another entire script right there and then, as if I'd not gotten one two days previously. THAT was a fun week. They didn't ask for the patches back either. So just used small amounts to potentiate the oxy. Got absolutely shitface wasted for the week using what was basically a free script and a few fent patches chucked in to boost the effects with, which it did at least, not completely suck at.)

But working on a small scale for analysis is better in every way. You need less for the samples to test, you waste less material, and if something is either highly potent or else highly poisonous, there is less risk to the chemist. And for the melting point determination, it means being able to keep it confined within a thin column and see it the moment it begins to 'sweat', that is to say, when a substance starts to develop a sheen, looks like moisture on the surface of the crystals or powder, resin or whatever else it might be, that can give further assistance to assaying the purity, under the magnifying glass.

Lestat:
Anyone know any good hosts for large videos? it's going to be just under 100mb, most likely, once converted from .mov to .mp4


As for latest projects, I think I just found one.

And thinking...I am getting SO pissed off with my doctor.

Basically the problem is, I want to get on a specific med, memantine, for a lesser known use (actually it does a whole bunch of useful things, ), really fixes my executive issues, overloading, and does a pretty damn thorough number on opiate tolerance, lowers existing tolerance, slows development of further tolerance, and more or less eliminates both the psychological reinforcing effects, and either stops or drastically lowers physical withdrawal effects)

The doc in question is a decent guy, and after I showed him and explained a few journal articles on the stuff, and my past personal experience with it, he's up for the idea, but there seem to be two problems, one-he's forgetful and two, seems like some kind of approval from some sort of specialist is needed for the off-label use. And since it's taken me several years even to get the GP to agree, and despite keeping reminding him, he either forgets, or whoever has to sign off on it either forgets, can't be arsed or never got the message (since I assume an outright refusal would be communicated to me) I've been waiting..fucking hell, I can't even remember. A good long portion of last year, at the very least.

So, decided to say 'fuck it', and make the stuff. Just been doing some digging, and found a rather useful journal article, plus plenty of chinese suppliers for the starting material they used, 1,3-dimethyladamantane, followed by bromination and a rearrangement to 3,5-dimethyladamantane, conversion to the acetamide followed by reflux in acetonitrile (methyl cyanide, a polar aprotic solvent with, unlike many other polar aprotics, a decently low boiling point, making it easier to strip off after) containing either sulfuric or phosphoric acid. But apparently the yields are not too good for large-scale synthesis.

But it involves a 6 hour reflux with LARGE quantities of bromine, not the nicest sort of task to have to undertake, as bromine is volatile, corrosive (I have some I made a while back from sodium bromide, by passing chlorine gas through a saturated NaBr aqueous solution, and distilling off the side product, bromine monochloride, although it was on a relatively small scale, ounces of Br2. And I DON'T want to have to do that on a scale fit to provide the liters of Br2 that I'd need for the scale I want to work at [about 1kg to begin with, that way, I can tell my doc 'sod the waiting, got enough for the next 10 years or so, as I'm tired of being fucked about and kept hanging', besides, thats the minimum order of most of the companies I'd have to get the precursor from]. Producing that much Br2 would be a real shitter of a job. I could do it, no doubt about that, but the byproduct, the BrCl is NASTY stuff, a golden yellow gas, quite a nice looking colour actually, but it's war-gas level toxic and most lubricants for glassware joints would be destroyed by it. I've still got two condensers and a flask fused together, from distilling iodine monochloride, ICl being a volatile liquid.

AFAIK BrCl is more hazardous than iodine monochloride, and being gaseous, rather than a distillable liquid that can be stored [I've got some in my hazmat fridge, and the ONLY way I'm able to store it, is in glass bottles that have a teflon cap, with a flexible teflon seal underneath, which compresses when the cap is tightened to prevent the vapours escaping, and wrapping the screw-threads on the bottle in a thick layer of teflon tape] And whilst the small amount of BrCl produced during the bromine synthesis was easily disposed of, I don't want to have to deal with it on a production-level scale, because fuck me, the interhalogens are all reactive as hell, viciously corrosive to pretty much anything they can't set on fire/cause to violently explode, including most greases/lubricants, water-reactive devils to handle, and toxic as blazes. I had an accident, once, with the friendlier relative, ICl, after the gas mask I was wearing slipped the non-return valve, causing it to just pull in the ambient atmosphere, I detected a very faint halogen-like odour, somewhat like iodine, but different in it's own way, not at a concentration that caused any immediate coughing or irritation (something like chlorine or bromine fumes have enough warning properties that if someone has a choice, and assuming it isn't some huge industrial spill big enough to incapacitate someone straight away, that one will instinctively back off. The ICl didn't, not at the levels I was exposed to, which amounted to tiny traces diffusing through the silicone based lubricant I managed to find that would survive the stuff, and the minuscule gaps between the ground glass surfaces of the joints. Could just barely smell it, got one little whiff of extremely dilute ICl vapour and ran like hell.

Hours later, I could barely breathe, wheezing, choking, spent the next week and a bit using an asthma inhaler I got scripted. Was a close one, could easily have put me in hospital had I not run for it, knowing the toxicity of the stuff. Or had there been any larger concentration when the mask broke, it could well have killed me. Stuff eats plastics other than teflon and similar resistant fluoropolymers like nobody's business, I tried using plastic keck clips at first during a distillation of ICl, to secure the ground glass joints, and they lasted maybe 10-15 minutes before crumbling, cracking and falling to pieces. Stainless steel ones fared a little better, somewhat less than 24 hours. BrCl isn't nearly so tame and liquefying it for storage isn't an option I'm willing to try, as it boils at 5 'C, and being so unholy corrosive, I'm no way trying to pressurize it in a cylinder, as it'd doubtless eat through it and explode, releasing a fucking crapload of lethal gas into the neighborhood.

Reactive isn't even the word when dealing with interhalogens, I've read some downright scary things about the fluorinated ones, such as a spill of chlorine trifluoride burning (and I don't mean melting/corroding, I mean actually causing it to burst into flames) through three feet of concrete, then setting about a meter of gravel and earth ablaze before it finally burnt itself out)

But the same paper details a route with much higher yields, they still start with the same precursor and rearrange to a 3,5-dimethyladamantane skeleton, via bromination, but I've found some more suppliers that actually have the required 3,5-dimethyladamantanyl-1-bromide in stock, and that a high-yielding two-step process can be used to prepare memantine, first step being refluxing with formamide, then refluxing the formamido derivative of the intermediate in concentrated hydrochloric acid. Yields are apparently almost quantitative for the formamido intermediate, and they got a 74% yield of the end product.

Looks like it'll cost a minimum of £100 for the 3,5-dimethyl-1-bromoadamantane for 1kg, but with the improved process, I'd put that down as worth it. Will give me a good reason to put my relatively new 10-liter 4-neck round bottom flask to use. 

Shouldn't even need to buy the formamide, well, I'll be able to test the reaction, certainly, on a smaller scale, then scale up (in this case, surprisingly, it'd be the formamide that'll prove my limiting reagents, at 100 quid a kilo for the 3,5-dimethyl-1-bromoadamantane. It can be produced by careful thermal decomposition (overheating, past 150 'C will decompose the formamide produced into a pretty unpleasant witch's brew of ammonia, carbon monoxide and hydrogen cyanide) of ammonium formate. Something I happen to have on the way, actually, although can produce more with ease now the 85% formic acid has arrived (just mix garden fertilizer, lye (ammonia evolution and lots of it on initiation of the reaction with a little water, water being added slowly from an addition funnel) to prepare a gas generator. Ideally to produce a concentrated solution of formamide, and strip the water under vacuum.

Queen Victoria:
Short version: What I'm cooking Julia Child wouldn't approve of.

Genesis:
What's the likelihood of Boris Johnson being Donald Trump's Doppelganger?

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