Author Topic: Short Question Thread 2.0  (Read 5707 times)

Tsathoggua

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Re: Short Question Thread 2.0
« Reply #120 on: July 17, 2012, 04:50:20 PM »
Morphine can form salts with bases, as well as with acids, the acidity of the phenolic functionalities enable it to form morphinate salts, and that of calcium is insoluble in water. So as far as I can see, simple basing of a filtered solution with Ca(OH)2 should allow the goods to precipitate. Then I'll have to see how to go about removing (and of course saving) the codeine for other uses, because codeine causes such a degree of histamine release that IVing it can cause pulmonary oedema.

Thebaine too, is toxic. Its an  antagonist at the strychnine-sensitive glycine receptor, like strychnine, or tutin. But I don't want to remove it, as in small quantities, it, like strychnine is also stimulant. And it changes the character of pod tea. Which is, having experience with both, quite different to (oral)morphine, codeine, and mixtures of the two.

So, really, what Toady wants, as his end reward for hard work well slaved over, is an ALMOST full spectrum isolate. Pod tea, minus the codeine. So he can pull out a little propionyl chloride, and make something that makes H look like any other boring opioid, despite how good it is in comparison to many.

This particular amphibian is fortunate enough to A-bee able to buy codeine, DHC, and morphine without a RX, as well as, if its still sold,  although I have not looked for quite some years, due to the former housemate (the Whore-Queen from Hades) being SEVERELY allergic to opioids from the morphine family. To the point of 'take an 8/500 co-codamol and die in minutes. She found out from a hydrocodone script in the US, luckily, it was one of those free samples docs give out to you lucky yank fucking bar stewards.

Luckily for it, that is. Not so much for this half-amphibian, half hymenopteran, half damn good looking goth/metalhead (well of course!) clastically autistic medical/neurochemistry/org.chem/mycology/(ethno/entheo)botany geek and 11 tenths math teacher (dyscalculia is about as desirable as an enema made from a slurry of wasp stings, rusty razor blades and thallium in a solution of HF in muslim piss...he has thought since he was first given a formal diagnosis that if it were not for being autie, he just would not ever have made it as either a chemist, or the extremely well read* mycologist and [ethno/entheo]botanist he is, he would without the slightest doubt have sold all his plant compendiums, medical textbooks, field guides to fungi, as well as the ones too detailed for field guides by age 6, and sold all his lab kit&chemicals by age 9 or so [the age he had enough to have anything worth selling, when he was much younger, of course he had no income of his own, and sadly his folks were not amenable to requests for birthday/xmas presents that consisted of strong acids, bases, pyrophoric reagents like LAH, white phosphorus etc., and sadly he had no net connection either to learn from, being in a school for Kanner's autistic kids and those with mental retardation, the 'science lessons' were unworthy of the name. Christ alive....to think! he has actually suffered the indignity there of being 'asked' to put his chemistry textbook away and circle the pictures in a worksheet like a good little kid! Toady could have flayed that teacher's parents alive for the offense of giving birth to a moron of that caliber])

Dyscalculia though, that can't be overcome by willpower, it will always be there, and unlike anything else about his neurotype, he would have that cured, and really wishes it were possible. It has made my life crowbegotten bastardly well hard since I first walked through the doors of a playgroup/playschool

(what is  called a a nursery school' in the US, 'oi you bloody cunt, gimme yer fucking wallet you bollock-nibbling son of a thousand syphilitic muslim fecal pellets'' in scotland, 'och aye gizzadrink', in ireland 'any chance of two of what the scottish man had?  a 'creche' over the pond, '*deafening sound of rushing air, WERE ARE ALL GOING TO DIE! ''QUICK! rush that bloody bastard!, but just make sure not to shake It , or for the love of god, yes, god(and/or gods), not muhammid! press that read spot in the middle of it's ugly little head; that sets it's vest off'' ALLAH BE PRAI...., *squelch*, *earsplitting bang*' in almost all of the middle east. 'kinderzimmer' in german,  and a 'hole scraped in the fecal matter top layer of the ground and the dirt beneath it' in africa):P


Makes more than you would imagine  so much harder than you imagine, not just math, but computer (in)security, medicine, electronics is a real BASTARD, school has been perdition lite edition for life, especially having no formal dx, getting a job that doesn't involve selecting something from one's self-taught skills and putting it to work wallet-stuffing, and (engineering+chemistry) is his self-employment :P)

As soon as a prospective employer sees that he has the worst possible grade in the lowest available qualification type in his country, they probably couldn't be paid to piss on his boots to give them a shine.

Thanks, bubble! any practical experience is worth a ton of theory, which can always bee downloaded online if one looks hard enough, for any endeavour though, once one has read some theory, and understood it, somebee's actual attempts are worth infinitely more (likewise if one is a lazy shit eater, which toady isn't. The only things he would eat off a spoon, opioids not in consideration, are would be held in the hand of his stalker :))

'ye know what they say 'a bong full of skunk is worth fiver worth of bush ;D'

Morphine content is low in bog standard pods, something like 300mg/100g of average pods from the UK climate, and no potentiators, other than a shot of IV clonidine, and some oral baclofen&pregabalin, (which would get Toady where he wanted to be twice (the 300mg morphine sulfate that is, not the pods, per os, unless a decently chosen cocktail of potentiators, enzyme inhibitors and the like were chosen and dosed non-too-stingy, assuming he wasn't withdrawing from his oxycontin script that is.

Toady had a feeling it may well bee the case that the pods would  yield something as foul to work up, as pods are to the nose, taste, and uggh!, sensory perception. The sensation of dried pod latex on his hands/fingers is a festering abomination of the worst kind.

Waxes, resins etc. are some of the nastier things to have to deal with in an extraction that aren't actually toxic.
Nomen mihi Legio est, quia multi sumus

I'm hyperbolic, hypergolic, viral, chiral. So motherfucking twisted my laevo is on the right side.

bubble

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Re: Short Question Thread 2.0
« Reply #121 on: July 17, 2012, 05:37:14 PM »
hey Tsathoggua,
That morphine will form the phenolate with bases is right, but jon posted in another topic that, if you concentrate your morphenate solution you will get alot of pseudomorphine because of autooxidation in a basic milleu. You are right that thebaine is toxic, but in the amount in the solution it's not that dangerous. Many alkaloids like narceine or thebaine or noscapine in the poppy tea have a synergy with morphine.

In a few days ( i think friday) i will post how to get a full spectrum of alkaloids from papaver somniferum. Because the way with the calcium morphenate is not the best one to get a full spectrum. the phenolate is way better to get only the morphine. So I am trying to make a better extraction for the full spectrum which is also my aim.

EDIT: my fan is broken so evaporating the solution will last much longer than with a fan. so i think i will have some results on monday..


« Last Edit: July 17, 2012, 09:22:37 PM by bubble »

fresh1

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Re: Short Question Thread 2.0
« Reply #122 on: July 18, 2012, 03:40:46 PM »
does anyone know of a test, other than a M.P,  for mono acetyl morphine ? (6 MAM) specifically?

Or any tests of a similar type to say a marquis reagent, which reacts differently for 'different' opiods?



btw. down here they grow a poppy very high in thebaine and very low in morphine...having eaten many grams, fresh can attest that it has a minimal opiate effect, however it also has, as best I recall, it seemed to initiate virtually no histamine release. No itchyness, red eyes etc. :-\

that said, the reason they want poppies high in 'thebaine' is becoz it is easier to convert into codeine or oxycodone, as the worldwide demand for codeine in so many formulas being much greater than that for morphine.

Quote
Table 1. World consumption in kg of the main narcotic drugs in 1995

Opium alkaloids and derivatives                  Synthetic narcotic drugs

Codeine    181,421                              Dextropropoxyphene    252,483
Dihydrocodein    27,340                        Pethidine    15,104
Morphine    15,594                               Tildine    8,529
Pholcodine    9,089                              Diphenoxylate    6,490
Hydrocodone    8,869              Methadone    6,337
Ethylmorphine    2,689
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Tsathoggua

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Re: Short Question Thread 2.0
« Reply #123 on: July 19, 2012, 08:36:08 PM »
Use it...make some fucking GOOD stuff!
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I'm hyperbolic, hypergolic, viral, chiral. So motherfucking twisted my laevo is on the right side.

Gypsy

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Re: Short Question Thread 2.0
« Reply #124 on: July 23, 2012, 06:37:36 AM »
Right so a 10liter ptfe drum was used similar to the one Electro´S suggested. A plumbing fitting was found with threads on the outside and inside, with the inside being 2mm smaller than my condenser size. the fitting screwed tightly into the mouth of the drum. The excess thread was removed on the inside as to provide better contact with the glassware.

To a 500ml RBF is added 20g piperonal, 16ml nitroethane, 6.42g ammonium acetate, and 55ml GAA. This is refluxed gently, with moderate stirring, whilst keeping the temperature in the 100 degrees region. This is allowed to proceed for two hours, after which the heat is removed, stirring maintained, allowed to cool to room temperature. This solution is added to 1500ml H2O with a light scattering of ice. 23.5grams of light-yellow mdp2np is filtered off, and washed with 20ml ice water, and allowed to dry overnight. This was used as-is, without purification, for the reduction.
23.5grams mdp2np was dissolved in 400ml hot MeOH, whilst 240ml GAA, and a further 100ml MeOH (80ml + 20ml wash) containing 1.5grams mercuric chloride is heated to to 60degrees Celsius. 45grams THIN aluminium foil was cut into small squares and placed into the blender, and added to the 10 liter ptfe drum, fitted with a leibig condenser. The HOT piperonal, GAA and mercuric/meoh solutions were added to the drum, which was mixed with a hershberg style stirrer, attached to a drill. The reaction started quickly, generating allot of heat. A wet towel was not needed to cool the drum down. A further 100ml hot MeOH was added over the course of the next hour. Once all the aluminium had broken down, the reaction generates even more heat and tons of foam, this is the reaction peak. Once the reaction was completed, a thick cement like layer was present, no aluminium foil remained. 500g NaOH in 1500ml dH20 was added with strong stirring. 1 liter of toluene was added, mixed and extracted. This was followed by another 3 extractions of 250ml each. The last extraction had a slight hint of color left, but I called it a day there. Extracts were combined and washed with 500ml saturated NaOH solution. The product was extracted into 1 liter 10% HCl solution, then basified with 500g NaOH, once again extracted with 3x150ml Toluene. This was then dried over Calcium Chloride, and gassed with anhydrous HCl.

On the first gassing it yielded 13grams! Infinitely better yield! Its so white and pretty haha. Feeling pretty happy with myself at this point in time.
Thank you again all, and good day!
« Last Edit: July 23, 2012, 06:53:54 AM by Gypsy »

Gypsy

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Re: Short Question Thread 2.0
« Reply #125 on: July 23, 2012, 09:21:00 AM »
Thanks for the heads up reckless! ;D

carl_nnabis

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Re: Short Question Thread 2.0
« Reply #126 on: July 23, 2012, 10:36:17 AM »
or maybe use sodium sulfate thats pretty easy to make anhydrous again too after use? i prefer sodium sulfate, but it should rest a half day for good drying results, truely a disadvantage vs calcium salts..
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Gypsy

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Re: Short Question Thread 2.0
« Reply #127 on: July 24, 2012, 05:14:25 AM »
not too worried at all about replenishing them. They're dirt cheap.
Anyway will collect some calcium oxide today instead.
looking forward to running the reaction again to confirm results!
...then a new project is needed  :D

carl_nnabis

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Re: Short Question Thread 2.0
« Reply #128 on: July 24, 2012, 06:43:11 AM »
short question, would reaction of 6-bromohexanoic acid with acetic anhydride suffice to give 7-bromomethylpentylketone?

Br-CH2-CH2-CH2-CH2-CH2-CHO-CH3
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4studiesonly

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Re: Short Question Thread 2.0
« Reply #129 on: July 26, 2012, 12:58:42 PM »
Is there any fun to be had with the shitload of bupropion-tablets of different kinds in my cupboard?
I mean chemistry-wise....
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carl_nnabis

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Re: Short Question Thread 2.0
« Reply #130 on: July 26, 2012, 02:00:25 PM »
hmmm you could reduce them using zinc to 3-chloro-n-tert-butylamphetamine... i dont expect more than a even easier seizure inducing and maybe an antidepressant effect from it?
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carl_nnabis

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Re: Short Question Thread 2.0
« Reply #131 on: July 26, 2012, 04:42:42 PM »
I have discolored 2-Methyl-2-Octanol a product from a grignard, but its badly discolored i dont want to apply a vacuum just for this because it has a high boiling point. Would swirling with activated carbon suffice?
Or no way to get around the use of a vacuum destillation?
Another option would be to form a solid ester that can be recrystallized, like a phenylacetic or benzoate ester i guess
edit: distilled twice and clean  ::)
« Last Edit: August 03, 2012, 01:33:15 PM by carl_nnabis »
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DopeBee

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Re: Short Question Thread 2.0
« Reply #132 on: July 30, 2012, 08:51:20 AM »
Right so a 10liter ptfe drum was used similar to the one Electro´S suggested. A plumbing fitting was found with threads on the outside and inside, with the inside being 2mm smaller than my condenser size. the fitting screwed tightly into the mouth of the drum. The excess thread was removed on the inside as to provide better contact with the glassware.

To a 500ml RBF is added 20g piperonal, 16ml nitroethane, 6.42g ammonium acetate, and 55ml GAA. This is refluxed gently, with moderate stirring, whilst keeping the temperature in the 100 degrees region. This is allowed to proceed for two hours, after which the heat is removed, stirring maintained, allowed to cool to room temperature. This solution is added to 1500ml H2O with a light scattering of ice. 23.5grams of light-yellow mdp2np is filtered off, and washed with 20ml ice water, and allowed to dry overnight. This was used as-is, without purification, for the reduction.
23.5grams mdp2np was dissolved in 400ml hot MeOH, whilst 240ml GAA, and a further 100ml MeOH (80ml + 20ml wash) containing 1.5grams mercuric chloride is heated to to 60degrees Celsius. 45grams THIN aluminium foil was cut into small squares and placed into the blender, and added to the 10 liter ptfe drum, fitted with a leibig condenser. The HOT piperonal, GAA and mercuric/meoh solutions were added to the drum, which was mixed with a hershberg style stirrer, attached to a drill. The reaction started quickly, generating allot of heat. A wet towel was not needed to cool the drum down. A further 100ml hot MeOH was added over the course of the next hour. Once all the aluminium had broken down, the reaction generates even more heat and tons of foam, this is the reaction peak. Once the reaction was completed, a thick cement like layer was present, no aluminium foil remained. 500g NaOH in 1500ml dH20 was added with strong stirring. 1 liter of toluene was added, mixed and extracted. This was followed by another 3 extractions of 250ml each. The last extraction had a slight hint of color left, but I called it a day there. Extracts were combined and washed with 500ml saturated NaOH solution. The product was extracted into 1 liter 10% HCl solution, then basified with 500g NaOH, once again extracted with 3x150ml Toluene. This was then dried over Calcium Chloride, and gassed with anhydrous HCl.

On the first gassing it yielded 13grams! Infinitely better yield! Its so white and pretty haha. Feeling pretty happy with myself at this point in time.
Thank you again all, and good day!

Is there a reason why so much mercury is used? Does this reaction need to run so hot and fast?

Would it be wiser to use 200-300mg Hg salt and maybe even an addition funnel to drip in a nitropropene solution.
« Last Edit: July 30, 2012, 09:05:00 AM by DopeBee »

Gypsy

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Re: Short Question Thread 2.0
« Reply #133 on: July 30, 2012, 09:54:41 AM »
Is there a reason why so much mercury is used? Does this reaction need to run so hot and fast?

Would it be wiser to use 200-300mg Hg salt and maybe even an addition funnel to drip in a nitropropene solution.

Only reason I used so much mercury was to ensure complete amalgamation quickly, as it was not washed and preprepared. I've found adding a little excess really helps. As for the fast & hot reaction. My yields have doubled. It would appear that its a bad idea to reheat the reduction to kickstart it again, which has happened to me upon addition of the remaining aluminium a few times. loss of energy I guess. Best to make sure you have plenty headroom. The foam in the reduction in the 10liter drum at one point was 7x as high as its starting level.
http://127.0.0.1/talk/index.php/topic,2962.msg32486.html#msg32486  (6  grams)
vs
http://127.0.0.1/talk/index.php/topic,2962.msg32646.html#msg32646 (13grams - the one you quoted)


DopeBee

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Re: Short Question Thread 2.0
« Reply #134 on: July 30, 2012, 08:14:22 PM »
Is there a reason why so much mercury is used? Does this reaction need to run so hot and fast?

Would it be wiser to use 200-300mg Hg salt and maybe even an addition funnel to drip in a nitropropene solution.

Only reason I used so much mercury was to ensure complete amalgamation quickly, as it was not washed and preprepared. I've found adding a little excess really helps. As for the fast & hot reaction. My yields have doubled. It would appear that its a bad idea to reheat the reduction to kickstart it again, which has happened to me upon addition of the remaining aluminium a few times. loss of energy I guess. Best to make sure you have plenty headroom. The foam in the reduction in the 10liter drum at one point was 7x as high as its starting level.
http://127.0.0.1/talk/index.php/topic,2962.msg32486.html#msg32486  (6  grams)
vs
http://127.0.0.1/talk/index.php/topic,2962.msg32646.html#msg32646 (13grams - the one you quoted)

How far up did the foam get? Like halfway?

Gypsy

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Re: Short Question Thread 2.0
« Reply #135 on: July 31, 2012, 06:15:11 AM »
was about 3 liters worth of drum space that wasnt full of foam. after a while I just sat there vibrating the drum gently, this broke up the foam with ease and kept it all at the bottom. But turn your head away for a minute and youre gonna want that headroom.

Electro´S

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Re: Short Question Thread 2.0
« Reply #136 on: July 31, 2012, 06:54:38 PM »
Hi all.
Could be THF substituted for Ethyl Acetate in the Sodium Stannite reaction from the Nitroalkene to the Ketoxime???

A facile ketoxime preparation. Varma & Kabalka.

hxxp://www.erowid.org/archive/rhodium/pdf/nitroalkene-stannite-1.pdf

One more time, Thanks again!!!  8)

T-cowboy

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Re: Short Question Thread 2.0
« Reply #137 on: August 03, 2012, 03:46:43 PM »
i dont think so, ethyl acetate might undergo a unwanted reaction in the stanite reaction after reading some refs, but maybe im off.

can i ask what you want to do with the ketoxime?

amide maybe? then a hofmann?

Electro´S

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Re: Short Question Thread 2.0
« Reply #138 on: August 04, 2012, 01:15:23 AM »
I don't want to do nothing...
But Zinc/ammonium formate is a good option for the amine in decent yields.

Zinc/ammonium formate: a new facile system for the rapid and selective reduction of oximes to amines

hxxp://www.erowid.org/archive/rhodium/chemistry/oxime2amine.zn-af.html

Tsathoggua

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Re: Short Question Thread 2.0
« Reply #139 on: August 04, 2012, 09:51:40 AM »
Very nice, electro. Toady is going to have to have a play around with that reaction, it looks most promising on paper. And FAST!, most rxn schemes going to completion in five minutes or less..
Nomen mihi Legio est, quia multi sumus

I'm hyperbolic, hypergolic, viral, chiral. So motherfucking twisted my laevo is on the right side.