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Author: Subject: What reagent would you like to see an illustrated guide for?
len1
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[*] posted on 28-7-2008 at 19:02
What reagent would you like to see an illustrated guide for?


Im looking for new syntheses to perform. If you would like to see an illustrated procedure demonstrated for a useful chemical reagent I would gladly consider writing it. Essentially Im looking for chemical reagents, which are useful, not instantly availale, whose procedure for manufacture is lacking in standard texts (in detail, purity analysis, kinetics etc.), is not drug related. CS2, SO3, Na were perfect past examples - have you any ideas of some more?

[Edited on 29-7-2008 by len1]
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octave
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[*] posted on 28-7-2008 at 19:49


Aldol condensations! Many useful chemicals can be prepared from this process. Though I cannot think of any chemical right off the bat I would love to have a pictorial of this reaction mechanism.

[Edited on 28-7-2008 by octave]
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Magpie
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[*] posted on 28-7-2008 at 20:22


I think there must be quite a few difficult to obtain reagents that are normally made on an industrial scale and which do not have readily available laboratory methods. I think those you have already mentioned fit that description. Two more that come immediately to mind are phosphorus and CCl4. In time I'm sure I can think of some more.

Also consider the reductants sodium borohydride and lithium aluminum hydride. And the Lewis acid AlCl3. There are also some on this board who would just like to make con H2SO4 without going thru SO3.

Edit: And my favorite, pyridine. :D

[Edited on 28-7-2008 by Magpie]
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UnintentionalChaos
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[*] posted on 28-7-2008 at 20:26


Well, Sauron has detailed Carbon tetrachloride quite a bit, but an illustrated guide would be excellent.

I'm sure there'd be an audience for phosphorus, although I wouldn't blame you for shying away from it due to a number of less than savory uses...

You could always tackle hydrazine...useful for precious metals reprocessing and syntheses such as luminol among other things.

EDIT: Magpie beat me to the posting. AlCl3 and borane/borohydrides would also be great.

[Edited on 7-28-08 by UnintentionalChaos]




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kclo4
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[*] posted on 28-7-2008 at 20:32


Personality I think a Ketene lamp would be really cool. Perhaps it isn't the hardest thing, but I've never seen a real one and eventually I would like to make one. there is always a setup for it and a sketched picture of the lamp, but never the real thing. Plus, ketene seems like a very useful chemical. Mostly because it can be used in place of Ac2O or make Ac2O from GAA. Ketene is pretty dangerous, but I think making it and using it would be a lot safer then phosphorous and a few other chemicals.
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Magpie
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[*] posted on 28-7-2008 at 20:32


I thought about hydrazine myself, but I think Mr Anonymous has given us the procedure in a thread on this board, although it is not as facile as an illustrated guide would be. Also, a synthesis for hydrazine sulfate does exist in Inorganic Synthesis, volume I.
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kilowatt
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[*] posted on 28-7-2008 at 20:35


Some very useful reagents that come to mind are thionyl chloride, nitrosyl chloride, PCl5. Even nitrites like NaNO2 don't seem to have many good lab synthesis methods out there. Precious metal salts and acids are good too. Borate esters are another good one.



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kclo4
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[*] posted on 28-7-2008 at 20:48


Mentioning Precious metals, How about an extraction of Pt/Pd from catalytic converters? or perhaps a decent Nickel Catalyst and a demonstration of what they can do?
Not to sure how many uses it has, and its not really that hard to make but I've read a few things on some of them and lately I've been pretty interested in them. I've been dissolving some nickel to try it out with something.

They seem to have pretty good potential.
http://www.erowid.org/archive/rhodium/chemistry/urushibara.h...
Here is a bad example of what one can use them for :S
http://designer-drug.com/pte/12.162.180.114/dcd/chemistry/am...
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DJF90
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[*] posted on 28-7-2008 at 23:53


Reducing agents like LAH and NaBH would be great! How about nitric acid from ammonia? And thionyl chloride, without using SO3... Wikipedia states that the reaction SO2 + Cl2 + SCl2 => 2SOCl2 is one method, which i think would probably more easily achieved for the home chemist than the SO3 methods. Maybe also preparation of sodium/potassium cyanide, as cyanide salts can be rather useful in organic chemistry, forming nitriles and the like... Other possibilities include making some sort of apparatus for catalytic hydrogenation, but using hydrogen produced from a reaction like 6NaOH + 2Al => 2NaAlO3 + 3H2, and finding some way of getting the hydrogen to a pressure of 3-10 atm or higher. "Freebase" hydrazine is a good idea, as azides could also be formed by reacting with a nitrite.

Personally some inverstigation into the SOCl2 reaction I posted or LAH/NaBH would be preferred :P
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Picric-A
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[*] posted on 29-7-2008 at 01:05


could you show some simple processes used in organic chemicstry for begginers?
eg. fisher esterification, dehydrogenation etc...
good luck with it!
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YT2095
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[*] posted on 29-7-2008 at 01:11


personally I would love to seea Diphenyl Oxalate synth using Phenol and oxalic acid as precursors.
maybe via transestrification of diethyl oxalate (that you would also make).




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[*] posted on 29-7-2008 at 02:01


Here are some that come to mind and are not stated by others: Making soluble relatively pure salts of chromium and nickel from stainless steel. Route to phenol starting from turpentine. Making benzene from something better available than benzoates.Use of ion exchange resins to make dilute acids from salts especially if electrolytic or some other easy regeneration of exchangers is possible. Electrolytic chlorine generator which can actually be used for chlorinations.

[Edited on 29-7-2008 by chromium]




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stoichiometric_steve
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[*] posted on 29-7-2008 at 03:36


LAH please :)



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Klute
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[*] posted on 29-7-2008 at 04:57


A low-pressure hydrogenation apparatus is a good idea, I'm starting to make a fewplans on making on to go up to 3 atm. Although it could be easily made from stainless steel, a thick hydrogenation bottle, etc, there are safety issues that need great attention, welding must be done very carefully and I guess there are alot of construction considerations.

With such an apparatus, catalysts like raney nickel (which usually performs very bad a atm pressures), Cu, etc could be very usefull for a great number of reductions.

Organic sulfonic chlorides, from the sulfonic acid and S2Cl2, for example, or chlorination of alkyl thiosulfates or sulfides could be very interesting too.
These could lead to preparation of safer alkylating agents, by reacting them with alcohols, which I think are a constant 'graal' :). Sulfonates could also enable one to perform various displacements.
Trialkylphosphates, from P2O5, or POCl3 from P2O5, etc all could be very usefull and a certain challenge (especially the oxychloride)

I think it's extremly generous on your part to ask memebers of the forum what they would like to see being done!

What ever your futur plans, good luck with it!




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[*] posted on 29-7-2008 at 10:52


A suggestion for len1 would be to add a synth, which also can be done by the moderately equipped home chemist. Chemicals requiring such intermediate apparatus and skills can still be very interesting for the average home chemist. Some to name:
- vanadyl salts like VOSO4.xH2O from pottery grade V2O5
- titanium salts from the metal and easy to obtain acids (e.g. TiCl3)
- luminol from naphthalene, phthalic acid or phthalic anhydride




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len1
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[*] posted on 29-7-2008 at 14:44


Thank you very much for your suggestions. Surprisingly the list of preliminarily ideas I jotted down got almost completely covered - CCl4, NaCN, NaN3 etc - so I was thinking on the right track. Some of the suggestions I have'nt thought of at all and will have to read up on, such as what Klute posted. Other things I thought you could readily buy, such as LiAlH4 and AlCl3 - ill have to ring up. Thank you
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[*] posted on 29-7-2008 at 14:55


Readily buy LiAlH4?? and where abouts do you live:P?!
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[*] posted on 29-7-2008 at 16:21


I'm with YT on the phenyl oxalates:

Oxalyl chloride and 2,4-dinitrophenol to give DNPO. The DNP we can do, the oxalyl chloride is a bit trickier. Of interest, oxalyl chloride (which Sauron has discussed quite a bit) can be directly oxidized with H2O2 in the presence of a fluorescent dye (i'm using perylene and rhodamine 6G) to yield chemiluminescence.

The PClx needed to make the oxalyl chloride would make this an interesting (if intensive) multi-step process that yields a rather nice chemiluminescent compound.

I have been making these (DNPO, TCPO) from oxalyl chloride and could document the procedure if anyone is interested.

Let's see, what else... Diborane, definitely. Anything with NaK. Reformatsky? LDA enolate formation. Sodamide (maybe not such a good idea, these days). Diazomethane. Magic acid. Some reactions using PTC to enable classical reactions in water. Ionic liquids.


Cheers,

O3




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[*] posted on 29-7-2008 at 17:54


Len.. I was thinking that since your very adept at manufacturing apparatus for chemical reactions, like your sodium cell, in my opinion it would be far more entertaining for the audience for you to stay with things that require skill in that area. The hydrogenation apparatus that Klute suggested or the ketene lamp that kclo4 proposed would be such a challenge. Anyone of us can toss some stuff in a flask and stir. The things that you build are quite amazing.

Regards,

Ord




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[*] posted on 29-7-2008 at 18:10


I second ordenblitz' suggestion. I would like to see a design for a homemade Parr reactor. Something that could be used for high pressure and high temperature reactions. Possibly even equipped with a temperature indicator, pressure indicator, and mixer. The design could then be verified by making a useful reagent that's difficult to obtain.

Today on the History channel a scientist was attempting to simulate conditions at the bottom of the ocean near hydrothermal vents. He used a metal screwed cap cylinder placed in a tube furnace. Attained pressure was several hundred atmospheres.
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Klute
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[*] posted on 29-7-2008 at 18:30


Indeed, a hydrogeantion apparatus would be very usefull! But considering the hazard, i think that the construction of a some what low pressure vessel first might be safer, to be able to notice the potential problems, and how these would go with higher pressures. A bit like starting a small scale reaction before scaling up :)

Higher pressures means cheaper catalysts too :) I wonder what things like Cu/SiO2 and Ni/C could do even at 3 atm, and if they could rival with expensive palladium and platinium...

Ah, i could do with such an apparatus right now, trying to mono-methylate that !@*รน#$ b-phenethylamine...




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[*] posted on 29-7-2008 at 20:07


Heck! I had not thought of that one, but a reliable home-brew hydrogenation apparatus would definitely be a winner.

I have wondered about using a bi-phasic system under pressure with H2 generation in-situ? I suppose you might need a flocculant to keep your catalyst where-you-want-it.

Cheers,

O3




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[*] posted on 29-7-2008 at 20:33


Some moderate to high temperature syntheses would be good to see too, and I think they would go well with len1's skills (this is one of my favorite areas of chemistry). For example CaS, CaC2, SO3 from the Contact Process, SO2 from calcium sulfate reduction, elemental silicon from silica and carbon, etc. Some of these require electric arc or oxy-fuel temperatures, but those can definitely be done at home with a little ingenuity.

Another thing that comes to mind is boron trihalides from halogen and boron trioxide/carbon at moderate temperatures.

I'm not sure if this still falls under the category of reagents, but some low temperature stuff would be interesting too, and I don't recall ever seeing a home chemist do it. I have always wanted to make a simple sterling or pulse-tube cryo-refrigerator (it does not seem outside the amateur scope at all, using modified compressors or lawnmower engines) for liquefying nitrogen, oxygen, natural gas, crystallizing dry ice, etc.




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Magpie
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[*] posted on 31-7-2008 at 11:36


Len, I remembered an old thread that is related to your question. If you need any more ideas take a look at:

http://sciencemadness.org/talk/viewthread.php?tid=1359&p...

[Edited on 31-7-2008 by Magpie]
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[*] posted on 31-7-2008 at 14:27


N2H4, KNO2, CaC2, HCl (from a chloride and H2O at high temp), H2O2, CaO2, Al powder (from molten Al and steam), SnCl4.
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