Even if some linear chain extension did take place as a side reaction, presumably nothing that couldn't be fixed either by vacuum distillation assuming there are no azeotropes, which for an old fashioned and short lived drug like this, probably weren't tested for extensively if at all; of course, or else fractional crystallization or column chromatography of the alcohol itself, derivatized as a solid carbamate fr.ex.
And cheap as chips, available starting materials are in any case, the aim, at least to come up with a synthesis reproducible by others, since unlike myself, there will be an awful lot of hobby chemists who have to fund and build their own lab, and whilst not all, some of their reagents and solvents need to be DIY'ed, etc., this, is why he needs first and foremost, to come up with something that can be done in a manner as facile as for example, the synthesis of chlormethiazole from thiamine (bisulfite cleavage, discarding the HIGHLY toxic convulsant nasty pyrimidine fragment, and washing thoroughly and repeatedly before proceeding with the chlorination, as well as vacuum distillation of chlormethiazole base, after the intermediate alcohol is halogenated with SOCl2, or, as he's been meaning to test out, PCl5, as well as use of the Appel reaction, triphenylphosphine/carbon tet as chlorine donor, since although he has a script for the stuff, although not here licensed for the indication, to control his seizures, which it does both well and fast as shit spews from the mouth of Donald Trump during one of his public diarrhea-exchanges, he has a rather enthusiastic liking either for chlormethiazole or bromethiazole, so finding alternate halogenating agents, like CCl4, CBr4, PCl5 and PBr5 to stand in for thionyl halides, which aren't the easiest of reagents to make, what with needing oleum or sulfur trioxide, and difficult to purchase, particularly thionyl bromide, as most places carry SOCl2, but much fewer also carry SOBr2, and I personally, have no shortage either of red phosphorus, of white, if I want it, in multi-kg quantities when speaking of red P, the more routes and procedures, the better, no?)
But for this particular drug, the methylpentynol, MeLi is out. Most clandestine chemists or tinkering hobbyists, even those who could safely handle an organolithium alkyl, would find it very difficult either to purchase or to make themselves. More so than grignards, for sure. How many, out of all the clandestine chemist professionals, and hobbyists put together, could, do you think, simply place an order for some MeLi as a calibrated solution? or if not, both make it themselves, and then keep what they have wrought, rather than have their MeLi burst into flames?
It is not, one can say with certainty, a reagent which lends itself to being scavenged from photo chemicals, fertilizers, pool treatments and removers of foot-fungus. Which, while he's more than happy to switch routes if something more practically facile and useful turns up after doing his best to get the Na or Li-acetylide based route up and running and OTC'ed so far back, it's hobnobbing with chlorobutanol, chloral hydrate and paraldehyde for next-door neighbours, for personal consumption if more expedient, he does need to find, as part of the point of the exercise, a viable route using alkali metal acetylide reagents for the ethynylation. since sodium metal, or lithium are not unobtanium-based reagents generally speaking, especially with the pyrometallurgical process Nurdrage came up with, using 1,4-dioxane to melt the fine dispersion of Na in a Na/MgO aggregate from a magnesiothermic reduction of NaOH or KOH etc. and coagulate the results into useful chunks of metals, with the dioxane itself of course being readily available, if one prepares it from scratch, starting with ethylene glycol and sulfuric acid. It's basically a thermitesque reaction, so not rocket science, but with the potential to bring alkali metal acetylides to the hungry, acetylide-starved masses using alkali metals solvated in anhydrous ammonia (if redneck hicks can make their NH3, since they can't ALL be stealing it off farmers, then so can bees who desire a honey to be supped from parts of the comb less well travelled, by way of oldarse wallbanger GABAergics that went the same way as the dinosaurs, Given it isn't actually OTC as such, but needs to be liquefied from the anhydrous gaseous ammonia using a dry ice/acetone bath after precooling using salted ice/glycol/methylated spirits/H2O mixture to spare on the dry ice, dry ice is orderable online freely enough for it to qualify as 'OTC' for the purposes of the establishment of a facile route to methylpentynol as an exercise in OTC-ing, for the use of others, and for the enjoyment of taking things right back to basics, and turning out something useful and hopefully pretty recreational from the likes of boxes of lawn fertilizer, caustic soda, tanks of acetylene or else generating it from calcium carbide (buyable, or makeable from quicklime and carbon at high temperatures) and H2O (if anybee has problems getting access to H2O, it's probably time for a career change, if they live long enough to do so
), and sodium metal, MEK, MEK being buyable easily enough, inexpensive, whilst sodium metal if a given bee cannot purchase it, then it isn't unmakeable, and advantageously producible from the magnesiothermic reduction slag, once powdered under argon in a blender, before being added to a flask of dry 1,4-dioxane, or even electrolysis of one stripe or another, on hydroxide, chloride etc. if one has to endure the finnicky-ness of electrolytic routes to alkali metals, rather than a simple if slightly exotic thermite composition, grinding the slag and refluxing under dry dioxane..
And even if one can't order dry ice, it could be made by exhausting inverted CO2 fire extinguishers through fine cloth then compacting it into bricks with blunt force and a mold so as to prevent it's overrapid evaporation and ease the burden of effort the totally OTC-bound chemist must go to in order to condense their anhydrous ammonia, so it's OTC, if filed under OTC-intermediate effort and difficulty/high cost per unit if made with fire extinguishers.
Surely, you can see his reasoning behind the exercise in mind, can you not? both for the enjoyment of being able to achieve the synthesis of an improvement on alcohol as sedative-hypnotic, which compared to ethanol, it pretty much has to bee, let's face it, ethanol is a shite drug, what more can one expect from one that is governmentally sanctioned and profited from
, starting from bare-bones materials such as any aspirant may achieve production of or obtaining thereof from really simple chemicals that even an american could hope to get OTC, hell, even an englishman such as myself!, Turning fertilizer, paint stripper, bog cleaner and antifreeze, some welding gases etc. into a proper alcohol worthy of consideration for consumption as a recreational, as a comedown-antidote for stimulant users, is part of it, but it's also the spirit of things, it's enjoyable to spend some days working in the back garden, generating the anhydrous NH3, etc., and enjoyable turning caveman-chemistry into actually functional, useful goods that shit on the likes of chloral or chlorobutanol (again, what doesn't!), with the knowledge that those of us who cannot buy OR make OR handle alkyllithium reagents even if they did get any, can still decide they want to try the alcohol in question, and actually go ahead and do so, using chloral hydrate-level resources and skill demands, or at worst, the kind of resources and skills required for a meth cook (not like generation of anhydrous liquid NH3 is new to clandestine chemistry, likewise it's going to have plenty folk already trained enough to handle the use of an alkali metal in liquid ammonia.)
It's just like cooking pizza from scratch, sure, if you've got 20 quid, you can ring for a takeout with all the toppings you want, but if all you have is pepperoni, cheeses, black olives and the flour to make dough, then you've got to make your own, in times of no money (pepperoni and black olives just happens to be the example because it's His favourite pizza
), but even if one HAS the money to buy a pizza and have it delivered, sometimes, one goes and makes themself a pizza, rolling and kneading the dough themselves, not because they must, but because they like to cook, and they like to cook in more ways than opening a cardboard box and stuffing the result in a microwave for 2 minutes on high. Because they CAN. Because they can do so, and because they'll have fun doing it, without resorting to cheating, like for the spirit of the proposition in question, using alkyllithiums would. That'd be like buying ready-made pizza dough complete with a bag of mozzarella and a jar of pickled olives with pre-cut pepperoni slices, as opposed to making one's own dough, and letting it rise, then baking it.
Yes, in this case, the fundamentals, like NH3 must be made, rather than dial-a-takeout, but there are allowances to be made for the OTC-er, it doesn't have to be strictly speaking something one may just walk up to a shelf in a shop and pick up a tank of, rather, one starts with fertilizer and caustic base, drying over quicklime or more NaOH, and dry ice, ordered or made, that is fair game though, making non-OTCs simply from OTCs.
And hey, it means more chemistry to get one's hands dirty with, which is in LC's book, somewhat of a directly proportional analysis of the fun to be had, plotted into a graph curve. The more, and the more simple one can engineer things such as for others of a less spoilt lab supplies selection to pick from, who CAN'T just go 'oh I want some methyllithium', then the more of a contribution, IMO has been made towards helping drive the vile drug war with all of it's attendant evils and evil-doers, further towards endgame, where it is to bee eventually recognized by ALL as being unwinnable in terms of prohibition. And the more this aim is fostered, the better.
Sure, I might have the pick of my chemical suppliers, but I didn't always. I didn't in my preteen years when starting out as a chemist, so the OTC spirit remains a noble aim to me, and one dear to my heart, even if now, all I need do is contact one of my hook-ups and get me those fancy, luxurious reagents that everybee wants, but not everybee is fortunate enough to bee able to have. I *WAS* that reagent-hungry young bee still earning his wings once. Now, not so, I could probably buy the sodium acetylide for example, but I don't want to buy it, not when I can go through the process of preparing the anhydrous liquid NH3, preparing the sodium metal (which I'll do, despite the fact I have it in bricks, covered in heavy paraffin, then heat-sealed under vacuum in a thick plastic liner, itself placed inside another, outer liner of thick heavy-duty plastic, purged with inert atmosphere and then sealed. But, as with everything, it's going to come from as simple a source, even when other sources and routes are available, as can bee. Not just for my personal fun in the exercise, but for all the other bees without connections, anyone looking to earn his or her wings and know how to use that stinger and to biosynthesize their favourite venom of choice and file off the barb on said sting to make sure they don't rip their insides out for a demonstration of stinging prowess.
For all those who once he was, this is a large part of why.
