Author Topic: Short Question Thread 2.0  (Read 5704 times)

Electro´S

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Re: Short Question Thread 2.0
« Reply #300 on: February 09, 2013, 01:23:14 AM »
A strange route to Amph was found in some where.
It was something like...
Benzaldehyde + Nitromethane => Nitrostyrene.
Nitrostyrene + NaBH4 => Phenyl-Nitro-Ethane.
P-N-E + Monometylation with Formaline => Phenyl-Nitro-Propane.
Phehyl Nitro Propane => Zinc/HCl.

What you think about it???
Is possible the monomethylation to "Nitropropane"?

It sounds like a dream, Nitrostyrene route to Amph or P2P  without Nitroethane.

Happyman

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Re: Short Question Thread 2.0
« Reply #301 on: February 09, 2013, 01:56:26 AM »

Quote
Lol, you're not going to get acetyl chloride from alanine and bleach.

I'm as lost as you, but sure did feel like an acid chloride when a gaseous white smoked filled my lab. Also present in solution was calcium carbonate, calcium hydroxide, magnesium sulfate heptahydrate, calcium chlorate, not like that explains anything...

lugh

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Re: Short Question Thread 2.0
« Reply #302 on: February 09, 2013, 04:17:18 AM »
Quote
does anyone have a write up for a Strecker Degredation of alanine to acetaldehyde, preferably with an easy to get oxidation agent like bleach.

The sodium hypochlorite degradation of alanine was published in Deutch by Langheld in 1909, and doesn't seem to be available freely online  ;)  A similar procedure using sodium hypobromite in English is attached  ;)  The end results from the effort applied 8)
Chemistry is our Covalent Bond

Happyman

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Re: Short Question Thread 2.0
« Reply #303 on: February 09, 2013, 09:44:25 PM »
Thanks! Hopefully I'll have a write-up soon.

lugh

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Re: Short Question Thread 2.0
« Reply #304 on: February 10, 2013, 10:37:18 PM »
Quote
I also now read about dehydration of ethanol at ucc.ie/academic/chem/dolchem/html/comp/ethanol.html and that yielded me
"When ethanol is mixed with concentrated sulphuric acid with the acid in excess and heated to 170 degC, ethylene is formed."
But i wont heat the mixture, so? And then from same source.
"When ethanol is mixed with concentrated sulphuric acid with the alcohol in excess and heated to 140 degC, diethyl ether distills over".
But again i wont heat the mixture so?

It all comes down to this (i now think, learning as i am writing this), is the production of diethyl ether gonna happen at roomtemperature? What if one worked in lets say a freezer? I am grasping for hope here, but i guess there are none....
Is the patient dead yet?

The attached articles explain the reaction mechanism of the catalytic dehydration of ethanol  ;) You need to start studying instead of posting so many inane questions  ::) It's probably going to take a much longer time than you think to understand chemistry enough to achieve your goals  :-X  The end results from the effort applied  8)

Chemistry is our Covalent Bond

Tsathoggua

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Re: Short Question Thread 2.0
« Reply #305 on: February 11, 2013, 02:24:54 PM »
Anybody know the BP of diisopropyl disulfide?

And can it bee separated easily via distillation from isopropyl mercaptan?

(lol..oh boy, ol' toady is sure going to bee popular with the neighbors :P)

Looking into the use of isopropanethiol as a demethylation reagent for codeine. Apparently the yields are absolutely fantastic compared with the pyridine route. Up to 85-90% using iPrSH, compared with some 30-35% for pyridine. Only disadvantage of course, is that stomach-churning stench, which is awful enough to shrivel the hairs off the arse crack of old nick himself.
Nomen mihi Legio est, quia multi sumus

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

Whale

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Re: Short Question Thread 2.0
« Reply #306 on: February 11, 2013, 08:19:22 PM »
Boiling point:
175-176¡æ J and K Scientific
177 °C/mmHg Tokyo Chemical Industry Ltd
177 °C/mmHg Tokyo Chemical Industry Ltd
177 Tokyo Chemical Industry Ltd
177.2 °C Food and Agriculture Organization of the United Nations
From:hxxp://www.chemspider.com/Chemical-Structure.70322.html

The boiling points are ~50c away from each other so it shouldn't bee a problem. Hope this helps! :)

%1

b6baddawg

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Re: Short Question Thread 2.0
« Reply #307 on: February 12, 2013, 07:15:52 PM »
I wanted some relatively pure lead II acetate.

Starting from lead metal would it be best to first form lead nitrate and decompose by heating then once the solution is syrupy from evaporation  add acetic acid?

Or would going directly by dissolving lead metal in acetic acid with hydrogen peroxide give lead II acetate trihydrate what could be used?

was to try a destructive distillation of propionic acid with benzoic acid + lead II acetate to yield propiophenone.

Wizard X

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Re: Short Question Thread 2.0
« Reply #308 on: February 12, 2013, 10:38:39 PM »
I wanted some relatively pure lead II acetate.

Starting from lead metal would it be best to first form lead nitrate and decompose by heating then once the solution is syrupy from evaporation  add acetic acid?

Or would going directly by dissolving lead metal in acetic acid with hydrogen peroxide give lead II acetate trihydrate what could be used?

was to try a destructive distillation of propionic acid with benzoic acid + lead II acetate to yield propiophenone.

Lead acetate can be made by boiling elemental lead in acetic acid and hydrogen peroxide. It's also possible to create with lead carbonate or lead oxide.

http://en.wikipedia.org/wiki/Lead(II)_acetate#Production

An aqueous solution of lead(II) acetate is the byproduct of the 50/50 mixture of hydrogen peroxide and white vinegar used in the cleaning and maintenance of stainless steel firearm suppressors (silencers) and compensators. The solution is agitated by the bubbling action of the hydrogen peroxide, and the main reaction is the dissolution of lead deposits within the suppressor by the acetic acid, which forms lead acetate.

Other Ref: http://www.sciencemadness.org/talk/viewthread.php?tid=5490
Albert Einstein - "Great ideas often receive violent opposition from mediocre minds."

Tsathoggua

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Re: Short Question Thread 2.0
« Reply #309 on: February 12, 2013, 11:25:29 PM »
Thanks for the info on the disulfide.

Toady apologizes for not just going to look it up himself, his only excuse, was that the computer he was using was not his own, since his keyboard is currently buggered, and in need of a replacement, he had to post the question right as the person who's computer was beeing used wanted it back, so Toady had only just the time to quickly post his query as to the BP of the disulfide and thiol while logging out of the places he had open; so not begging for spoonfeeding, just a matter of practicality and having to post as quick and concisely as possible.

Thanks. 

Of course, the alkyl disulfides aren't going to smell too pretty, although nothing like as foul as mercaptans. Toady has (unfortunately) had a previous experience with the smell of thiols, in just about the worst possible manner, having, a few years previous, a bit of a problem with GABAergic sedative abuse. Chlormethiazole being the drug of choice...and the steep dose-response curve aside (its much more similar in action to a barbiturate than a benzo, both subjectively and in terms of dose-response curve. It can be really euphoric in sufficient doses, but also pretty dangerous in overdose)

It appears, that in sufficient quantities one metabolic pathway involves producing some sort of mercaptan type metabolite, leading to Tsathoggua sweating, salivating, urinating, shitting, lachrymating the stuff, Hades, even his nasal mucosa were releasing said hideous stench in-situ.

No amount of showering, or shower gel could even come  close to removing that stench, while it was beeing produced in-vivo :P

Lol, people even crossed the street to avoid him while he was walking down the road.

No experience working with the purified compounds, although he has confidence in his ability. What he is wondering about more, is the disulfides, which will be produced as a byproduct.

Can anybody think of anything that could be done with diisopropyl disulfide? as it is, its just a byproduct, but Toady always likes to save potentially useful byproducts, in the hopes that they can bee turned to some use.

And how potent is the stink of these lower aliphatic alkyl (di)sulfides? not something toady has ever worked with before.                                                                                                                                                                                                                                                                                                                                                                                                                                                                                               
Nomen mihi Legio est, quia multi sumus

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

atara

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Re: Short Question Thread 2.0
« Reply #310 on: February 13, 2013, 04:31:52 AM »
Hi, does anyone have a write up for a Strecker Degredation of alanine to acetaldehyde, preferably with an easy to get oxidation agent like
bleach. I've ran the rxn about a dozen different times and just can't get a distilate. Vinegar was used as a  catalytic amount of acetic acid to prevent polymerization.
No write-up handy, but I'd try TCCA before I got all fancy-like.

Quote
A strange route to Amph was found in some where.
It was something like...
Benzaldehyde + Nitromethane => Nitrostyrene.
Nitrostyrene + NaBH4 => Phenyl-Nitro-Ethane.
P-N-E + Monometylation with Formaline => Phenyl-Nitro-Propane.
Phehyl Nitro Propane => Zinc/HCl.

What you think about it???
Is possible the monomethylation to "Nitropropane"?

Should work just fine; it's just another Henry reaction. However, you'll generate 1-phenyl-2-nitro-2-propene, which must be reduced accordingly (NaBH4). Also, it's kind of a pain in the ass...
« Last Edit: February 13, 2013, 04:37:55 AM by atara »

antibody2

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Re: Short Question Thread 2.0
« Reply #311 on: February 13, 2013, 08:43:25 PM »
If antibody were synth an oxime, she would freebase the hydroxylamine in situ using sodium acetate. But she has never reacted hydroxlamine with an aldehyde, usually do it with a ketone. What are you trying to make?

check these out
http://about.mdma.ch/000250280.html
http://www.erowid.org/archive/rhodium/chemistry/alhg.oxime.html

Good luck

The Lone Stranger

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Re: Short Question Thread 2.0
« Reply #312 on: February 16, 2013, 01:54:58 PM »
I have heard that in the EU they have lists of products with their contents that doctors in poisons units have so that they can help people who have imbibed them  ....... does anyone know where i can get that information and / or other information on the subject  ....... please .?

java

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Re: Short Question Thread 2.0
« Reply #313 on: February 16, 2013, 07:35:32 PM »
I have heard that in the EU they have lists of products with their contents that doctors in poisons units have so that they can help people who have imbibed them  ....... does anyone know where i can get that information and / or other information on the subject  ....... please .?

...this might help,


http://www.uq.edu.au/_School_Science_Lessons/topic19a.html#19.1.15


main page with diversity of information .....non related,

http://www.uq.edu.au/_School_Science_Lessons/
« Last Edit: February 16, 2013, 07:38:28 PM by java »
¡Prefiero morir de pie que vivir siempre arrodillado!.Emiliano ZapataIt is better to die on your feet than to live on your knees!.......

The Lone Stranger

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Re: Short Question Thread 2.0
« Reply #314 on: February 16, 2013, 08:00:04 PM »
Thanks Java .... looks interesting ...... but i want / need the details about a product and the variations of the ingredients between the same product from different manufacturers .  And at the moment i dont want to say what it is because if i do ...... before i can explain more ........ i might get shot and land in the shit posts section .......

Tsathoggua

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Re: Short Question Thread 2.0
« Reply #315 on: February 16, 2013, 10:29:13 PM »
Just bee aware, that when dissolving elemental Pb in the H2O2/AcOH mixture, it foams up.

Toady made some just the other day, for drying to the anhydrous salt, dissolving in alcohol then use for preparing H2S indicator paper.

Foams up...He tested on the scale of 1.5-2g or so of lead, made from roofing sheet, hammered into thin foil strips, and sliced to shreds using scissors, GAA, and 9% H2O2 (all toady had to hand, crappy over the counter hair bleach, as he is getting ready to do a two-tone blue dye job)

The resulting product bubbled up like the head of a beer, and ended up setting, like a sort of lead (II) acetate souffle
Nomen mihi Legio est, quia multi sumus

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

Happyman

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Re: Short Question Thread 2.0
« Reply #316 on: February 24, 2013, 11:48:24 PM »
Hi, does anyone have a write up for a Strecker Degredation of alanine to acetaldehyde, preferably with an easy to get oxidation agent like
bleach. I've ran the rxn about a dozen different times and just can't get a distilate. Vinegar was used as a  catalytic amount of acetic acid to prevent polymerization.
No write-up handy, but I'd try TCCA before I got all fancy-like.

The formation of the aldehyde is not a problem. Collecting it without forming an exotic derivative ( like 2,4-dinitrophenylhydrazone, oxime, ect.) seems to be impossible. Not even a dry ice cold finger will produce a distillate.

The total mechanism of the Strecker Degradation eludes me, but I'm under the impression that acidic environments yield the nitrile and basic ones yield the aldehyde. How do you plan to keep the solution slightly alkaline when using trichloroisocyanuric acid as an oxidizing agent?

fishinabottle

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Re: Short Question Thread 2.0
« Reply #317 on: February 26, 2013, 07:58:01 PM »
Hi, does anyone have a write up for a Strecker Degredation of alanine to acetaldehyde, preferably with an easy to get oxidation agent like
bleach. I've ran the rxn about a dozen different times and just can't get a distilate. Vinegar was used as a  catalytic amount of acetic acid to prevent polymerization.
No write-up handy, but I'd try TCCA before I got all fancy-like.

The formation of the aldehyde is not a problem. Collecting it without forming an exotic derivative ( like 2,4-dinitrophenylhydrazone, oxime, ect.) seems to be impossible. Not even a dry ice cold finger will produce a distillate.

The total mechanism of the Strecker Degradation eludes me, but I'm under the impression that acidic environments yield the nitrile and basic ones yield the aldehyde. How do you plan to keep the solution slightly alkaline when using trichloroisocyanuric acid as an oxidizing agent?
By adding a base to form a alkaline salt maybe? A frivolous idea I admit, but you might consider to read the TCCA relevant papers as I doubt your musings hold water in the light of the enlightening literature.
Sorry no time to do it myself at the moment.

/ORG

fishinabottle

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Re: Short Question Thread 2.0
« Reply #318 on: February 26, 2013, 08:08:59 PM »
Thanks Java .... looks interesting ...... but i want / need the details about a product and the variations of the ingredients between the same product from different manufacturers .  And at the moment i dont want to say what it is because if i do ...... before i can explain more ........ i might get shot and land in the shit posts section .......
MSDS or analysis paper from the manufacturer/wholesale/importer, thats, so health-relevant in the database which is not accessible by the public and does not allow the kind of searches you are thinking about. Usually no problem to aquire directly, if not for dl anyways a polite asking for it works wonders.
Of course they are all riddled with undetectable quantum mechanical tracking software and thousands over thousands outsorced dataslaves work 16/7 to mine this data to track YOU down. Now they have Bin Laden its only logical that YOU are next.
Beware!

/ORG

ImAMANGUYS

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Re: Short Question Thread 2.0
« Reply #319 on: March 03, 2013, 12:03:46 AM »
Hello  ;D

According to most peracid writeups/pictorials, its stated that the color of the mixture after peracidic addition and stirring will be an ORANGE or a RED. In my case, this doesn't seem to be true as after two hours of stirring my solution is only tinged YELLOW. I followed:

http://www.erowid.org/archive/rhodium/chemistry/peracetic.chromic.html

where Chromic states that:

Quote
If you decide to not use a cold-water bath, the flask will reach a reflux and the condenser becomes necessary. The color changes from a colorless biphasic solution to gain a very light yellow tinge. At the end of the reaction, the solution is dumped into a 1L sep funnel and 325ml of 5% NaOH is added. The funnel is shaken and let to settle. The DCM is kept and washed again with 5% NaOH. Then the DCM is distilled off and recovered for future use. 66.8g of glycol is recovered. (105% yield, this yield is likely a bit high as some of the glycol is likely the mono- or di- acetate ester)

Apparently his mixture also produced only a YELLOW tinge.

Attached is a picture of my flask after 2 hours of stirring. Have any other bees in this hive tried the buffered peracetic who could give me advice? If not i must wait until workup.

Thanks in advance :)