Author Topic: Short Question Thread 2.0  (Read 5708 times)

LilDookie

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Re: Short Question Thread 2.0
« Reply #220 on: October 15, 2012, 01:49:10 PM »
Hi guys, I used to be reDEEMed, but forgot my password and the email I used. So here I am, new name.  I have found myself playing with glass and chemicals again, but I'm a bit out of practice. I plan to do an oximation later tonight or tomorrow and had a solvent question. Have any of you ever used chloroform as a solvent in oximations? Normally I would use ethanol and have have decent luck with isopropyl as well. But I have never tried chloroform and I have a lot of it.
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newbiechem

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Re: Short Question Thread 2.0
« Reply #221 on: October 22, 2012, 04:23:35 AM »
crystals smelling like fish hehehehe
recrystalize in IPA would solve the problem?
peace

ImAMANGUYS

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Re: Short Question Thread 2.0
« Reply #222 on: October 23, 2012, 05:32:20 PM »
New question:

When using the bromosafrole method, how can you tell when the reaction has completed without decanting and testing in cold sulfuric acid? Is there a definite end color?

I've had my safrole in HBr for 20 hours and would like to keep itt in longer if it needs it. THANKS!

2bWinston

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Re: Short Question Thread 2.0
« Reply #223 on: October 23, 2012, 08:20:25 PM »
Im wanting a PTC, and OTC, has anyone had success with benzalkonium Chloride??? Its OTC, Any other ideas folks? 

http://en.wikipedia.org/wiki/Benzalkonium_chloride

« Last Edit: October 23, 2012, 08:28:49 PM by 2bWinston »

LilDookie

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Re: Short Question Thread 2.0
« Reply #224 on: October 28, 2012, 09:30:52 PM »
So, I been reading various patents for oximations and I see that the solvent must be carefully selected depending upon which base is used to liberate the hydroxylammonium and what it is you're trying to oximate (is that even a word?) and also dependent on other factors. I apologize for a post that is worthy of Vesp's board of shame. I'm self taught, as some of you guys may remember, and I took a year off. I didn't have access to my gear, also I got a bit burned out from my first year of study, which I gave everything I had. It was a very rewarding endeavor, not financially, but in terms of personal satisfaction it was worth every headache I got from balancing equations in textbooks and doing boring exercises online. I got a lot of good advice from you guys, and it materialized in the form of mundane compounds that were transformed into truly magical ones.

Sorry again for the lame question. If someone has a proverb or a parable that would help me understand the mechanism of oximations, I'm all ears. In the mean time, I'm off to read. Thanks for suffering me, guys :^D
The cost of sanity in this society is a certain level of alienation.
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Sneak

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Re: Short Question Thread 2.0
« Reply #225 on: October 29, 2012, 09:31:56 AM »
Welcome back dude and good luck.I followed everything you did and took it as some inspiration.I'm still learning though.same route
If you really want to enjoy a pure, clean product the only way... is to make it yourself...

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Tsjanga

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Re: Short Question Thread 2.0
« Reply #226 on: October 29, 2012, 04:04:44 PM »
Someone more info about DECARBOXYLATTVE OXIDATION UTILIZING PYRTIDTNE N-OXIDE from 1 of our favorite aldehyde?
Would love to see a route to another of our favorite honey.

Sedit

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Re: Short Question Thread 2.0
« Reply #227 on: November 02, 2012, 12:47:53 AM »
I'm still looking for a simple process for the reductive Methylation of Alkenes mainly Nitropropenes so any suggestions would be greatly appreciated.

I envision the production of various Amphetamines using Benzaldahydes, Nitromethane, reductive methylation and further reduction of the nitro group to Amphetamines to bypass the need for Nitroethane.
There once were some bees and you took all there stuff!
You pissed off the wasp now enough is enough!!!

EMTWC

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Re: Short Question Thread 2.0
« Reply #228 on: November 03, 2012, 01:52:51 PM »
has anyone ever strangled their assistant in the lab? That's not the short question.

Was in the final stages of step 3 in the brightstar synth (Rxn: Safrole -(Wacker Oxidation (PdCl2+Benzoquinone))-> MDP2P). The assistant was asked to mix up the 270 ml dH2O and 30 gm NaOH for the final washes. Turned around and they had dumped the lye into the DCM/organics and then proceeded to add the water.

PISSED!!!! FIRED!!! FUCK!!!!

So now there is this thick black liquid that doesn't look like it will separate. Is there any way to save the MDP2P?
roll some bones and catch a fire

lugh

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Re: Short Question Thread 2.0
« Reply #229 on: November 03, 2012, 06:07:50 PM »
Quote
So now there is this thick black liquid that doesn't look like it will separate. Is there any way to save the MDP2P?

It may take a long time:

http://parazite.nn.fi/hiveboard/methods/000220524.html

Flashlights have been used to detect the layers separating ;) There will probably bee some losses due to the Cannizarro reaction  :-X The end results from the effort applied  8)

Chemistry is our Covalent Bond

EMTWC

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Re: Short Question Thread 2.0
« Reply #230 on: November 13, 2012, 04:50:53 PM »

It may take a long time:

http://parazite.nn.fi/hiveboard/methods/000220524.html

Flashlights have been used to detect the layers separating ;) There will probably bee some losses due to the Cannizarro reaction  :-X The end results from the effort applied  8)

many thanks lugh. You are an invaluable resource to this community.
dumped in a bunch of dH2O, shook, and left it. flashlight, or more just holding at proper angle gave sight to layer separation.
There was DEFINITELY a reaction; Cannizarro we now know...
And there will surely be loses. Just washed the orgs with the appropriate NaOH/H2O solution. Started out with 156 gm safrole, presume to have about half remaining.

thanks again lugh!
roll some bones and catch a fire

Quantum Dude

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Re: Short Question Thread 2.0
« Reply #231 on: November 13, 2012, 05:10:16 PM »
Quote
So now there is this thick black liquid that doesn't look like it will separate. Is there any way to save the MDP2P?

 There will probably bee some losses due to the Cannizarro reaction  :-X The end results from the effort applied  8)




The Cannizaro reaction is limited to aldehydes lacking alpha-hydrogens so MDP2P is not prone to such an oxidation. However, it could, under the right conditions, undergo an aldol condensation.

EMTWC

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Re: Short Question Thread 2.0
« Reply #232 on: November 13, 2012, 05:40:48 PM »
looks like there is 147+ gm.
Given cold shaky hands during pouring, and just general sloppy first time at the rodeo syndrome, not too bad.

thanks lugh, and QD...
roll some bones and catch a fire

lugh

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Re: Short Question Thread 2.0
« Reply #233 on: November 13, 2012, 08:04:57 PM »
Quote
The Cannizaro reaction is limited to aldehydes lacking alpha-hydrogens so MDP2P is not prone to such an oxidation. However, it could, under the right conditions, undergo an aldol condensation.

Aldehyde by products have been identified in published wacker oxidation articles, but the old hive post that was loosely quoted in that reply was obviously in error slightlly since any such aldehydes would have alpha hydrogens  ;) The tar produced by both the aldol and Cannizarro reactions is certainly useless for our purposes ::) The chapter from House's Modern Synthetic Reactions on aldol reactions can be downloaded from:

https://the-collective.ws/forum/index.php?topic=19378.msg147825#msg147825

 8)
Chemistry is our Covalent Bond

Goldmember

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Re: Short Question Thread 2.0
« Reply #234 on: November 16, 2012, 08:51:02 AM »
Few quick ones.

For something to do,someone I know will soon attempt an AlCl3 catalysed Friedel-Crafts condensation of 1,4 Dimethoxybenzene with Allylamine in the hope of ending up with some 2,5 Dimethoxy (beta) methylphenethylamine? This person has no idea about pharmacology whatsoever...

1) Is anyone aware of any recent literature reports on the effects of this CAS listed compound, or its ring halogenated derivatives?
2) Anyone see why(chemistry wise)this scheme wont work?
3) Can any Pharmacologically minded Wasps suggest what, if any qualities this compound would possess?
4) Why is Pervitin considered an old school branding of (meth)amphetamine, yet in the scientific literature of the time i.e WW2 Pervitin was more often used to describe beta-methylphenethylamine?

Cheers.

Oh, Quick, simple,bulk FC catalysts can be prepared by grinding an excess of clean, oven dried Metal grit(turnings etc,not powder as it gos very fast) with TCCA and heating in an appropriate sized retort-condensation set-up, which has been swept with argon, or at least evacuated. Caution: the reaction is fast and furious and small scale(sub 10gm) experimentation is a must beforehand to see what power it is you need to contain.
Successfully used for production of anhydrous AlCl3 and FeCl3. No explosions yet...

lugh

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Re: Short Question Thread 2.0
« Reply #235 on: November 16, 2012, 12:00:46 PM »
The Friedel-Crafts reaction:

http://en.wikipedia.org/wiki/Friedel-Crafts

The chemical transformations that can be made with it are alkylations, acylations, hydroxyalkylation and sulfonylation  ;)  Thus the proposed Friedel-Crafts reaction can't occur   :P One can prepare ketones with an acylation, and then reductively alkylaminate the carbonyl group  :-X  This reaction is described very thoroughly in most organic chemistry textbooks and many articles   8)

Chemistry is our Covalent Bond

Goldmember

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Re: Short Question Thread 2.0
« Reply #236 on: November 16, 2012, 01:30:53 PM »
"The chemical transformations that can be made with it are alkylations"...

So what would you suggest as the name of the reaction I propose?
No seriously?;)
Are you reading a-LL-ylamine or a-LK-ylamine?

For similar examples Check US244518

or JACS article by same group: htxp://pubs.acs.org/doi/abs/10.1021/ja01244a049 (Same Authors as above)

or the references provided by Java in this SM thread: htxp://www.sciencemadness.org/talk/viewthread.php?tid=2974

Cheers


« Last Edit: November 16, 2012, 02:23:17 PM by Goldmember »

lugh

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Re: Short Question Thread 2.0
« Reply #237 on: November 16, 2012, 08:48:27 PM »
Quote
For similar examples Check US244518

The proper number for that patent is 2441518, 244518 is an automatic boiler feeding system by a man named Babbitt  ;) That's definitely a type of Friedel-Crafts reaction that's not covered in the textbooks or Wikipedia  :P Whether it's of any use to the swarm is yet to be determined  :-X The documents are attached for those that want to read them  8)
Chemistry is our Covalent Bond

Goldmember

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Re: Short Question Thread 2.0
« Reply #238 on: November 17, 2012, 04:15:13 AM »

The proper number for that patent is 2441518, 244518 is an automatic boiler feeding system by a man named Babbitt

Lol, oops sorry. Handy patent none the less.

Whether it's of any use to the swarm is yet to be determined  :-X

So no physiological reports that you know of? Or are you referring to that pimp ol` boiler system which is obviously an extremely useful reaction the swarm would find useful?

The documents are attached for those that want to read them  8)

Thanks for uploading those for us. I see my notions are as popular as ever.:)

Ill keep searching.

Oh 1 more quick one: Some iodine has been combined with mercury to form a beautiful crimson salt. Now this has been stored under acetone, as this has been found to be a convenient solvent into which aluminium wire can quickly be dipped, in order to amalgamate the surface for further reaction. Upon returning to this container after whatever period of time , the salt has turned olive colored. Any idea what causes this discoloration? Ive looked high and low for an explanation to no avail.
 Upon addition of a small amount of oxidizer(percarbonate or hypochlorite) the typical crimson color re-appears but again turns olive upon standing for some time. This has been observed in mixtures having not yet been exposed to Aluminium.

Confused?

The Lone Stranger

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Re: Short Question Thread 2.0
« Reply #239 on: November 20, 2012, 08:52:26 PM »
High girls ,

This one is for people that can understand german .

On another forum i was pointed at this ---- >

http://www.nachtschatten-science.ch/data/web_vorschau_phenethylamine.pdf

I was asked my opinion of it and replyed ---- >

"  At first glance i see nothing new there ..... except that its in german . I know very little about chemistry but from what i have read so far the only people that the chemistry there will interest is german speaking chemists that dont know anything about chemistry / psychoactive chemistry . All the information i see there is available directly or indirectly in PIHKAL , TIHKAL , the encyclopedia of psychoactive drugs and the encyclopedia of psychoactive plants .

Any psychoactive chemist weather above or underground already knows the chemistry there ...... or if he thought about a specific molecule that he had no experience with and then about the possible ways of changeing its structure it would be obvious . "

Is my answer crap ? Was i a dickhead ..... AGAIN ....... If so please tell me .

Thanks .

The hunting season is open ........ Fire free !!!!