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Author Topic: How are you feeling right now? (Pt 2)  (Read 167690 times)

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Offline Lestat

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Re: How are you feeling right now? (Pt 2)
« Reply #10365 on: October 09, 2017, 10:40:23 PM »
MMmmm QV. I bought what must be nearly 10 tubs of ben&jerrys peanut butter ice cream earlier today. Took me about 5 minutes to eat 4 of them, one after the other. Salty peanut butter-caramel with chocolate-covered lumps of frozen peanut butter throughout, and caramel sauce in a toffee-peanut butter salty and caramel-flavoured peanut butter icecream. Fucking lovely. Came with one of those foul coarse untouchable, unspeakably disgusting in a sensory molestation kind of way lolly sticks meant to be used as a spoon. So I gritted my teeth and used my knife to lift them off the top of the pots and flick the sticks into the bin without touching them or looking at them any more than I had to. Well not touching the fucking things at all. I can't BEAR those awful things. They are just fucking WRONGNESS. A befoulment even of parts of un-nature that have no right to exist in this universe, and a source of putrescent filth that pollutes the world just by their being present upon it.
Beyond the pale. Way, way beyond the pale.

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Offline odeon

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Re: How are you feeling right now? (Pt 2)
« Reply #10366 on: October 09, 2017, 11:59:01 PM »
Why does it have to be morning again?
"Only two things are infinite, the universe and human stupidity, and I'm not sure about the former."

- Albert Einstein

Offline "couldbecousin"

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Re: How are you feeling right now? (Pt 2)
« Reply #10367 on: October 10, 2017, 05:13:59 AM »
MMmmm QV. I bought what must be nearly 10 tubs of ben&jerrys peanut butter ice cream earlier today. Took me about 5 minutes to eat 4 of them, one after the other. Salty peanut butter-caramel with chocolate-covered lumps of frozen peanut butter throughout, and caramel sauce in a toffee-peanut butter salty and caramel-flavoured peanut butter icecream. Fucking lovely. Came with one of those foul coarse untouchable, unspeakably disgusting in a sensory molestation kind of way lolly sticks meant to be used as a spoon. So I gritted my teeth and used my knife to lift them off the top of the pots and flick the sticks into the bin without touching them or looking at them any more than I had to. Well not touching the fucking things at all. I can't BEAR those awful things. They are just fucking WRONGNESS. A befoulment even of parts of un-nature that have no right to exist in this universe, and a source of putrescent filth that pollutes the world just by their being present upon it.

  You mean popsicle sticks?  :orly:


   My mother hated coffee from paper cups that she could "still taste the trees in."  :laugh:
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Offline Charlotte Quin

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Re: How are you feeling right now? (Pt 2)
« Reply #10368 on: October 10, 2017, 06:14:45 AM »
Bronchitis/chest cold. A strange sort of cold that I've never really had before (I mean, a cold sans a blocked nose).
That explains the chest pains the other night - it was a precursor.

Offline Lestat

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Re: How are you feeling right now? (Pt 2)
« Reply #10369 on: October 10, 2017, 10:04:01 AM »
Its certain types, its the texture and the thought that goes along with them.  'magnum' ice-creams, I can't even touch the sticks, they are awful. Same kind. If I'm to eat the ice-creams I have to wear gloves and wrap the wrapper round the stick without touching it or its a sensory nightmare. These ice-cream pots left the exact same things on top like a goddamn boobytrap for autistics, the fucking monsters.

Hope you feel better soon CQ, I'd hug you but it'd probably hurt you and lead to me ending up with your ilness too.
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Offline Lestat

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Re: How are you feeling right now? (Pt 2)
« Reply #10370 on: October 10, 2017, 12:01:18 PM »
Elated, now my own rotavap is finally, FINALLY within reach after all these years. If I get really lucky after rent and food purchases. Then I'll have enough money left behind for me to buy myself some lithium aluminium hydride, as somebody recently  tipped me off to a supplier of all kinds of useful, often exotic and difficult to get hold of reagents and solvents that are often those which are extremely difficult to get. I previously, to get the lithium aluminium hydride I required, would have had to buy half a kilo for close to £400, and it doesn't have a great shelf life, needs EXTREMELY careful storage conditions, for it degrades easily, it is sensitive to oxygen in the air, it is sensitive also to water, including that present as traces of water vapor in the atmosphere.

And when it does so react, it may do so with extreme violence, giving off very rapidly, extremly large volumes of hydrogen gas and a lot of heat. It can, and when moistened from atmospheric H2O vapor, have the hydrogen take fire and then the LAH itself starts to burn, in an intense metal fire-like fire which is difficult to put out and burns very hot indeed. Requiring, in its use, glassware which has been dried in the oven by flame, sealed by a rubber septum, and the reagents transferred under pressure of inert gas, with dried inert gas used also to shield the reaction.

So naturally I want to buy that which I have immediate need of, and a little extra, for more reactions, but in quantities of maybe 50g-100g at most, that I can use quickly. The site in question even offers 10g quantities, suitable ideally for a single procedure. or two of them perhaps. Also Red-Al is available at good prices as a solvent dispersion, a usually very expensive reagent. And one I have been wanting greatly.

Being able to get 10g of LiAlH4 at a time is fucking excellent:D hoping I've enough left after paying rent and buying food, after buying myself my rotavap, to buy a little LAH as well. That will simplify my workup procedures and syntheses of certain targets And when I can afford it, I'll get myself some of the gentle, yet high-yielding and clean, and unlike LAH, non-pyrophoric hydride reducing agent Red-Al.

Oh boy, I'm fizzing with plans right now.
Beyond the pale. Way, way beyond the pale.

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Offline Phoenix

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Re: How are you feeling right now? (Pt 2)
« Reply #10371 on: October 10, 2017, 01:10:33 PM »
Tired. Stacked 3.5 cords of wood. Still have 6.5 more cords to go.
“To rise, first you must burn.”
― Hiba Fatima Ahmad

Offline 'andersom'

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Re: How are you feeling right now? (Pt 2)
« Reply #10372 on: October 10, 2017, 02:25:42 PM »
Rather crap, but the plumwine was nice.
I can do upside down chocolate moo things!

Offline Lestat

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Re: How are you feeling right now? (Pt 2)
« Reply #10373 on: October 23, 2017, 04:14:29 AM »
Just picked up my med refill, so after some oxy and chlormethiazole, pleasantly relaxed. And not at all displeased when i checked my bank balance and found £100 over a grand.
Beyond the pale. Way, way beyond the pale.

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Offline Queen Victoria

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Re: How are you feeling right now? (Pt 2)
« Reply #10374 on: October 23, 2017, 08:57:16 AM »
Nostalgic thinking about our dog Rusty.  (See another post)
A good monarch is a treasure. A good politician is an oxymoron.

My brain is both uninhibited and uninhabited.

:qv:

Offline Phoenix

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Re: How are you feeling right now? (Pt 2)
« Reply #10375 on: October 23, 2017, 01:54:31 PM »
Really tired and I have to stay up until midnight to pick up SO from work. :yawn:
“To rise, first you must burn.”
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Offline Lestat

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Re: How are you feeling right now? (Pt 2)
« Reply #10376 on: October 23, 2017, 04:22:21 PM »
*sends QV big hug and sends miss K a couple of lines of freshly made, guaranteed un-cut premium-grade amphetamine HCl, of the kind I'd consider good enough for myself, and guaranteed Hg-free, having been done via borohydride reduction of P2NP instead, followed by acidic iron dust/ferric chloride reduction in glacial acetic acid, plus a couple of his sleeping pill script for after your business picking up the SO is done so you can sleep easily after:) And a big hug too of course. Can't leave you out can I now?*
Beyond the pale. Way, way beyond the pale.

Requiescat in pacem, Wolfish, beloved of Pyraxis.

Offline Queen Victoria

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Re: How are you feeling right now? (Pt 2)
« Reply #10377 on: October 23, 2017, 05:52:23 PM »
Thanks Lestat.

Thinking I should not be over optimistic.  I've cooked dinner 2, two (count them) 2 nights in a row.  Just take it one day at a time.

BTW - they weren't lavish dinners:

Macaroni and cheese with hamburger (mince) bits
Red beans and rice
A good monarch is a treasure. A good politician is an oxymoron.

My brain is both uninhibited and uninhabited.

:qv:

Offline Phoenix

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Re: How are you feeling right now? (Pt 2)
« Reply #10378 on: October 23, 2017, 06:12:41 PM »
*sends QV big hug and sends miss K a couple of lines of freshly made, guaranteed un-cut premium-grade amphetamine HCl, of the kind I'd consider good enough for myself, and guaranteed Hg-free, having been done via borohydride reduction of P2NP instead, followed by acidic iron dust/ferric chloride reduction in glacial acetic acid, plus a couple of his sleeping pill script for after your business picking up the SO is done so you can sleep easily after:) And a big hug too of course. Can't leave you out can I now?*
I'm sure that is said with a lot of care, but for the non-chemists, it sounds like you're trying to kill me. :laugh:
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Offline Lestat

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Re: How are you feeling right now? (Pt 2)
« Reply #10379 on: October 23, 2017, 09:53:57 PM »
Actually it is quite the opposite m'ilady. Since a very popular reaction type for either reduction of P2NP, or reductive amination of P2P (phenylacetone) or reduction of phenylacetone ketoxime to amphetamine (in the last case) or methamphetamine (or ethylamphetamine for people with a preference for it) is reduction of the P2NP (1-phenyl-2-beta-nitropropene) or reductive amination of P2P (1-pheny-2-propanone/P2P/phenylacetone) with either an anhydrous alcoholic solution of methylamine (for methamphetamine) or ethylamine (for N-ethylamphetamine) or alternately, one can also employ nitroparaffins, nitromethane and nitroethane respectively for the same process, as the nitroalkanes undergo reduction of the nitro group to an amine, and in both cases the reaction proceeds via an intermediate imine, which is reduced to the alkylamine (I.e methyl/ethylamphetamine) and the way this is often done, is by preparing an aluminium amalgam, using aluminium foil, cut up into about inch-wide squares and folded up a few at a time very loosely into gently folded balls, and reacted with a solution of a divalent mercury salt, such as (most commonly) HgCl2, mercuric chloride (mercury (II) nitrate is the other commonly used salt although I have a hunch it ought to be less than ideal given that the reaction is a reduction, whilst the nitrate anion is an oxidizer) although how much effect this would have in practice is debatable, and more or less a personal musing of mine, since in an Al-Hg reduction only a very small amount of mercury (II) salt is used, sometimes, depending on the scale of the reaction, and the substrate, its just added off the tip of a knife point.

The role of the mercuric salt is to depassivate the aluminium, since Al is a very reactive metal and in the right conditions, a powerful reducing agent, and as such, being a powerful reducing agent it means its also very easily oxidized, and aluminium is just that. Once first exposed to oxygen it forms a very fine surface layer of aluminium oxide that, as its said, 'passivates' the aluminium, its only microns thick but it also near enough instantly reforms if damaged.

When Hg is present, it destroys this very thin passivating surface layer of oxide and allows reaction with the bare aluminium surface, and prevents the Al2O3 layer reforming, when used as an amalgam this allows the use of aluminium as a powerful reducing agent. The drawback of the Al/Hg is that mercury is very toxic, and a pollutant as well. And whilst the metal mercury itself is primarily toxic via the vapors, rather than bulk metallic Hg, (although the vapor pressure is actually significant enough, I've seen an ultraviolet photograph of mercury once before and it showed fumes billowing off like crazy) its a lot less hazardous than its salts, which being soluble are absorbed much more easily than mercury metal. And of the two common oxidation states, Hg (I)  [mercurous] is the lesser hazard, whilst mercuric (Hg (II)  ) salts are a LOT more toxic, HgCl, mercurous chloride or calomel, was used as a medicine in olden times although recognized as toxic even in some medical manuals of mine from the 1700s, the deadly nature of 'corrosive sublimate', as HgCl2 (mercuric chloride, the divalent chloride of Hg)  [Hg generally displays just the two oxidation states, apart from Hg (0), in mercury metal itself, the two being Hg (I) (mercurous) and Hg (II). (mercuric) and of the two, mercuric salts are FAR more toxic. Its probably the only item in my lab that actually causes me to feel fear working with it (HgCl2) and I've only maybe a few grams at most, or I did when I first bought the last lot I purchased, and less than that now, having used some). Stuff gives me the fucking creeps. Its just so damn toxic, I don't want anything to do with it if I can help it.

But there are other ways to deprive that particular felid of its epidermis. That do not involve mercury.

Such as for example direct reduction of the 1-phenyl-2-beta-nitropropene, that can be done in a one-step reaction, plus workup using lithium aluminium hydride, or in two steps using borohydride to reduce the double bond to give 1-phenyl-2-beta-nitropropAne, the saturated nitroparaffin, and then reduction of the nitro group using an acidic dissolving metal reduction, such as fine iron dust in hydrochloric or glacial acetic acid with some ferric choride hydrate added as a catalyst and the slurry mechanically stirred (since the iron is of course magnetic, one can't use magnetic stirring) from overhead whilst kept at 80 'C for 2.5 hours or so. This reduces the nitro group to an amine, forming amphetamine from 1-phenyl-2-nitropropane, and if the same reaction conditions are used on P2NP (1-phenyl-2-beta-nitropropEne) it undergoes a rearrangement as well as a reduction, to give the ketone, phenylacetone, 1-phenyl-propan-2-one, which can be used in several ways, either other methods of reductive amination after preforming the imine with an anhydrous alcoholic solution of methyl or ethylamine for meth/ethamphetamine respectivey, whilst using a suitable dessicant agent, since forming the intermediate imine generates an equal quantity (molar) of H2O, and the simple phenyl-2-iminopropanes are not stable against hydrolysis and the very water they produce as they are formed will destroy them unless the water be trapped, either by use of a dessicant, or by azeotropic distillation;

And then borohydride can be used to nicely cleanly reduce the imine in anhydrous iPA or most likely in THF or ether.

Or for plain un-alkylated primary-amine amphetamine from P2NP, you just employ the acidic iron/ferric chloride reaction to give phenylacetone, extract it with dichloromethane (aka methylene chloride, or dichlor for short, or else chloroform can be used also, but I prefer DCM, its cheaper and its boiling point is lower) and the DCM or CHCl3 washed with aqueous 10-20% sodium hydroxide (caustic soda) solution repeatedly until the color is discharged (it typically looks really dark when first done and the acid portion is really black looking or dark rusty orangey and thick, slurry like. But the DCM or chloroform easily extracts the P2P, and that separated off chlorinated hydrocarbon nonpolar layer repeatedly washed with the hydroxide, cleans it up, then the DCM/chloroform is distilled off, and ideally the P2P yielded thus is fractionally distilled under vacuum to purify it, although if not possible then the ketone can also be made into its bisulfite adduct using sodium bisufite or metabisufite in aqueous alcohol, crystallized out, due to its insolubility, and washed further with various solvents (ketone bisufite adducts are piss poor soluble in most solvents) and then can be regenerated to reform the ketone using a mild base such as sodium or potassium carbonate solution, and re-extracted into DCM, dried over sodium sulfate, magnesium sulfate etc. to remove the water traces,

Then the dessicant should be, if one is thorough in recovering as much as can be, washed with further anhydrous solvent to get the last bits of P2P, then the phenylacetone thus cleaned reacted with an alcoholic solution of hydroxylamine, to form the ketoxime, and after isolation of the oxime (distillation off of the alcohol, and washing free of unreacted hydroxylamine and unreacted base, sodium acetate working nicely enough to deprotonate the hydroxylamine hydrochloride or sulfate used, to allow it to react, in freebase form (you don't want to store pure, neat hydroxylamine freebase as its unstable and has in the past caused explosions in industrial plants, particularly when heated, so NH2OH salts are used instead, and deprotonated with a mild base to form the freebase in-situ at room temperatures or warmed and it reacts as soon as its formed thus averting explosions)

And the oxime, as with most ketoximes or aldoximes are insoluble as fucking hell in H2O, although they can be very difficult to crystallize indeed, but they can be used, as long as they are clean and pure, in their favourite state (I.e oiled out and desparately doing their damndest to stay as a thick oily viscous liquid-oily blob), as they are, without needing to crystallize the ketoxime, and it really is exceedingly difficult to crystallize even when very pure,

Oximes are just like that generally, but it doesn't matter, one simply makes sure it is free of H2O, then takes it into a solution in anhydrous ethanol, and reduces the phenylacetone ketoxime to the amine (amphetamine) by means of the Beaveault-Blanc reduction (sodium metal in anhydrous ethanol, the substrate being dissolved in the EtOH and then the sodium added carefully in small pieces, under inert gas, preferably argon, as its easier to form a protective blanket due to its being much denser than air, although nitrogen, or even helium, with care, can be used)

The acidic iron methods are clean, from a toxicological point of view, much nicer than mercury-based-anything.

The workup if going with the phenylnitropropAne is a bit of a mess, and theres always a lot of excess iron and iron oxide slop to be vacuum-filtered with fine filter paper, and plenty sour-smelling highly acidic slurry to process, but it is much safer than mercury reactions to work up. And the disposal of iron oxides and iron environmentaly speaking is not problematic, since its basically rust and iron ore, not deadly toxic Hg salts and Hg amalgam. The dichloromethane or chloroform are simply distilled off, washed several times with caustic solution and with brine solution and with H2O to neutralize the PH and redistilled for re-use (disposal into the environment is not a good thing, chlorinated hydrocarbons are bad ozone depleters and environmentally unfriendly so the prudent chemist recycles it wherever possible.

(and NEVER burns them, its alright for some solvents, hydrocarbons, ethers etc. but halogenated hydrocarbons can form some really nasty things when burning, such as phosgene (carbonyl chloride) or in the case of chlorofluorocarbons, fluorophosgene and hydrogen fluoride gas,

and these are singularly lethal, phosgene in fact having been used as one of the early chemical weapons in the days of trench warfare, as a replacement for and advance on chlorine gas, when gas masks that protected the soldiers from Cl2 gas were in wide use, carbonyl chloride (phosgene), was used as a replacement for chlorine gas, and unlike Cl2, which stings, makes one's eyes run like crazy nose run and sting, and makes you cough and is generally irritating at concentrations far less than are sufficient to be lethal. Phosgene on the other hand, C(=O)Cl2, carbonyl dichloride, has very, very little odor, and what it does have by way of smell, is not particularly alarming either, it smells of musty hay, faintly (I have smelled it, once, and the simple fact I did scared the fucking shit out of me, I thought I was a dead man still walking, since the effects of phosgene are delayed significantly after exposure by many hours often), and there is no irritant property to it, nothing to warn you whatsoever.

 The reason I am still alive, after accidentally producing a very small amount of phosgene one time is because, and ONLY because I knew what the smell is due to reading of the history of chemical warfare, so I knew what to be alert to, I smelled musty hay, faintly as can be, a mere hint, and I RAN for it, grabbing my gas mask on the way and slamming it on like there was no tomorrow. If I hadn't, there would not have been. Not for me, at least. After I got the mask on, I vented the lab, completely, opening every window, setting pumps up inside to suck in inside air and vent it out, setting up scrubber tanks, everything. And of course clamping down on, and stopping that reaction proceeding as fast as could be done and connecting the outlet of the container it was done in to a scrubber tank to destroy any further produced (accidentally, I'd NEVER deliberately produce phosgene, or use it as even a transient, in-situ generated intermediate in a reaction. Its just scary fucking stuff. Just thinking about that faint smell that day for the few seconds smelling that tiny trace is enough to make my hands shake, because that was too damn close. If I hadn't known my military history relating to the WWI-WWII periods I would not now be typing this post, as I'd have died of fulminant pulmonary oedema, drowning on dry land, with my lungs filling with my own blood plasma.

Thankfully, I am well read in a wide variety of subjects of all sorts, and I'm bloody quick on my feet when I have to react instantly to a hazardous situation of that kind, I've developed some nigh supernatural reflexes over the years since my childhood :autism:  When it comes to accidents involving either highly toxic substances, they very rarely happen, I am cautious by nature, in terms of my lab practices, careful and methodical. On the rare occasion something does happen involving a deadly toxin or spill of something corrosive as hell (or worse, both corrosive AND toxic,

When Murphy decides to be a bastard of a law enforcement officer that particular day :P) then I've got by any accounts quite some reflexes ingrained in me by dint of both much reading, and unlike my early forays as a kid into chemistry, much more learning and importantly, practical experience, so when it comes down to something un-preventable like a flask failure due to badly tempered glass, that could happen to anybody unfortunate, and resultant liter or two of boiling concentrated sulfuric acid and chromyl chloride at about 140-150'C being launched downwards as a flask literally splits in half with the bottom dropping out due to thermal shock, despite the glass being borosiicate, but  the individual piece being defective in its manufacture. Shouldn't happen, did. And if I'd been any slower, I'd have melted myself from the waist down. And melted my balls to carbon ash for sure, probably given myself cancer in as many places as a tumor could grow, and if not lucky, burnt my legs and waist down to bare bones, and maybe carried on going, whilst choking death on the CrO2Cl2.

As it was, I got away unharmed, with the only damage being the wooden bench being burnt to char, and saturated in hexavalent chromium dross, which had to be cut out of the bench with a saw, as if it were itself a malignant tumor, and a suitably shaped and sized slab of wood inserted and screwed in, whilst the chromium salts were carefully leached out of the wood-ash and recovered as much as possibe before the remainder and wood ash slops were sent for hazmat chemical disposal at the relevant section of the municipal waste dump as the toxic waste they were.



So, as for the two-step NaBH4 reduction of P2NP then Fe/acid/FeCl2 reduction to amphetamine, its a clean route, and the same route without borohydride, on plain P2NP to give the ketone, then oximation, or borohydride reductive amination, these are clean methods. Hg free. General moral-Hg is nasty in general and ideally avoided if at all possible. And you, miss K my dear, deserve far better than even the most meticulously purified product prepared via Al/Hg.

And besides, I don't like doing that reaction for any substrate, its temperamental, one time barely starting, the next taking off like a bloody cannon shot and only stopping near the top of several METERS of condensers. One time so slow as to need hotplate heating and a blowtorch, the next so rapid and exothermic that the flask needed periodic immersion in an ice-salt-antifreeze cryo bath to stop a Hg-slop flash-boiling and taking off like a fucking space rocket blastoff. Which needless to say, would splatter toxic slop everywhere that'd be a nightmare to clean. Especially the portion splattered on the ceiling.

Its also a shitbag to extract from, a shit to filter, and what is being filtered is a nasty slurry of hard-to-separate fine aluminia soaked in mercuric fucking chloride. In short, its the  next worse thing to bathing my sandblasted ball-sack in the remains of a freshly-dead ebola virus victim having been just ground to human hamburger in a woodchipper and blender. Al-Hg amalgam reductions really 'aren't my cup of tea' as we say over here. Never had much luck with them either. It just isn't a reaction that like me, any more than I like IT.
Beyond the pale. Way, way beyond the pale.

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