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Author: Subject: The short questions thread (1)
chemrox
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[*] posted on 2-2-2009 at 14:27


You could try some hardware store zeolites as molecular sieves to pull the last bit of water out. Have you checked the boiling pt? It should be elevated a bit by the water if there.



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[*] posted on 2-2-2009 at 16:42


What would the zeolites be marketed as in the hardware store? Just zeolite or is there a brand to look for?
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chemrox
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[*] posted on 3-2-2009 at 00:03


Zeolite.. they will be with the water purification materials. Also do a google for zeolite..
http://www.bearriverzeolite.com/brz-specifications.htm

[Edited on 3-2-2009 by chemrox]




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[*] posted on 3-2-2009 at 01:04


dryer cartridges for refrigeration fluids are an easily sourced source of zeolites. Danfoss is a large supplier manufacturing out of mexico i believe. Almost every suburb in the western world will have a refrigeration mechanics supplier as it is such an essential industry for food safety.



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[*] posted on 3-2-2009 at 11:20


Has anybody got any information of the synthesis of Hydrazine from chlorourea and sodium hydroxide?
I understand chlorourea can be made by passing chlorine through a soloution of urea with a suspention of ZnO (can CaCO3 be used instead of ZnO?)
I guess i could just acidify with H2SO4 to precipitate the sulphate from the reaction mix..
thanks in advance.
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Panache
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[*] posted on 3-2-2009 at 16:06


Does silver(II) form any volatile salt or complex at stp?
Are the ammoniated silver(II) complexes, that are reputed to be explosive, so sensitive and/or easily formed, that one should avoid any contact between ammonium solutions and silver(II) solutions or are the salts/complexes only explosive when dry?




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[*] posted on 3-2-2009 at 16:25


Yes, it forms a pyridine-complex, and it can be isolated as the peroxidisulfate salt:

http://www.versuchschemie.de/topic,11731,-Tetrapyridinsilber(II)-peroxodisulfat.html

If you can't read it:
-dissolve 15g K2S2O8 or 13,2g Na2S2O8 in 400ml water.
-Dissolve 4,5g AgNO3 and 5ml pyridine in 100mL water.

Add the solutions to eachother, a orange color is produced and precitipate is formed. Leave the solution to stand for 30min.
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[*] posted on 4-2-2009 at 00:18


Interesting thing about silver(II)-pyridine complex. Nice to try on a reagent tube scale.

@Panache: You are talking about ammoniated silver(II) complexes, but these are plain silver(I) complexes. If you mix ammonia and a solution of a silver(I) salt and allow to stand for a few hours, then a solid silver(I) compound (some amminie/nitride/amide complicated badly specified complex) is formed, which is extremely sensitive to mechanical agitation. Simply decanting the wet solid from a container may lead to an explosion already.




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stoichiometric_steve
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[*] posted on 4-2-2009 at 14:17


Are Swagelok threads a proprietary thing or is there a standard naming for it? I have a manometer with a 1/8" (or so i think, the small one) outer threading and i need to adapt it to a tube nipple. I haven't found anything so for that could do this.



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[*] posted on 6-2-2009 at 05:15


Quote:
Originally posted by stoichiometric_steve
Are Swagelok threads a proprietary thing or is there a standard naming for it? I have a manometer with a 1/8" (or so i think, the small one) outer threading and i need to adapt it to a tube nipple. I haven't found anything so for that could do this.


I haven't found anything that fits other than Swegelok stuff, however i have not asked the Swagelok rep directly, not that he would know neccessarily being a sales rep, lol. I try to avoid the system given the joins are not guaranteed once loosened and retightened (as compared to the Prochem system which is). Swagelok however do offer a full range of thread to nipple adaptors which could be ordered online easily enough.

Alternatively buy 20 old GC's for $20 and salvage the nipples.




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[*] posted on 12-2-2009 at 10:19


what componet will produce if water add to phenylacetyl chloride?



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[*] posted on 12-2-2009 at 17:12


^ Carboxylic acid will be formed. Phenylacetic acid.
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[*] posted on 13-2-2009 at 09:50


http://www.orgsyn.org/orgsyn/orgsyn/prepContent.asp?prep=CV1...

Is there any reason why the above reaction is not used more often in the preparation of nitrostyrenes? Granted, it is for unsubstituted benzaldehyde, but I can't see any reason why it isn't used in any, for example, 2c-h syntheses.

What about the 3,4,5 substitution pattern? It seems like it would be easier to use NaOH as the "catalyst" (though not finding a mechanism, I'd imagine that it proceeds through sodium methyl-nitronate) than trying to find/prepare some odd amine.




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[*] posted on 13-2-2009 at 09:56


Quote:
Originally posted by Intergalactic_Captain
http://www.orgsyn.org/orgsyn/orgsyn/prepContent.asp?prep=CV1...

Is there any reason why the above reaction is not used more often in the preparation of nitrostyrenes?

Maybe you just did not look hard enough. I have seen a few examples at the Hyperlab forum.




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[*] posted on 13-2-2009 at 10:04


The Hyperlab? Not speaking russian, I've never checked it out. Would you be able to give any examples of reactions tried and what the yeilds were?

...When I said it was not used often, what I meant was that in my beilstein searches I've not seen it more than a couple of times, and in googling and searching the old rhodium archives it's never come up (everyone seems to use EDDA).




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[*] posted on 14-2-2009 at 02:56


Quote:
...When I said it was not used often, what I meant was that in my beilstein searches I've not seen it more than a couple of times, and in googling and searching the old rhodium archives it's never come up (everyone seems to use EDDA).

So you are concerning the catalyst? Oh dear, there are many catalysts except EDDA. For example, ammonium acetate, cyclohexylammonium acetate. Alkalines will also do. Just google smth like " Henry reaction catalysts"
I thought first you did not find at rholdium any examples of henry reaction at all..
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[*] posted on 14-2-2009 at 17:00


I'm sorry am I reading this correctly? You didn't find examples of the Henry reax at Rhodium archives? No that can't be right. My question is in the Henry reaction between benzaldhyde and nitroethane have better catalysts been found since the Org Syn article posted by Nicodem? I seem to recall this being done with ammonium acetate but the mixture was kept in the dark for two weeks until yellow crystals of nitropropene formed.



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[*] posted on 14-2-2009 at 21:16


Is it possible to isolate the Schiff Base of a ketone such as P2P/MVK/MDP2P in order to get 100% imine formation, aiming to increase the yields of an Al/Hg reduction?

Formula409.
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[*] posted on 15-2-2009 at 08:27


HOw can ifigure out the size of a reflux column when refluxing in various size flasks and volume in flask,,,,,solo



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[*] posted on 15-2-2009 at 10:01


Quote:
Originally posted by Formula409
Is it possible to isolate the Schiff Base of a ketone such as P2P/MVK/MDP2P in order to get 100% imine formation, aiming to increase the yields of an Al/Hg reduction?

Formula409.


I see two questions here. Yes Schiff bases are isolated all the time before the reduction is done. With ketones you need a catalyst like p-toluenesulfonic acid. A few crystals.

Does that get you 100% yield? Usually not. The reduction doesn't always get you 100% and various methods require different workups that all have yield implications. You're planning on an aluminum amalgam redux? You will have some washing up to do after that.

[Edited on 15-2-2009 by chemrox]




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[*] posted on 15-2-2009 at 14:20


Is stainless steel resistant to oxalic acid?

Im evaporating a solution of oxalic acid in a stainless steel vessle and the solution is taking on a green color.

Is this from contamination or it the stainless under attack?

Ok I just changed to a glass evaporation plate and on a good note the solution wasnt what was green it just appeared that way because the stainless steel had turned green.

Have I lost some oxalic due to this or am I still good to go?

I am extracting out of a dilute rust remover solution and I was suprized to find oxalic crystalized nicely on the bottom as soon as I opened it but Im still awaiting the final yeild from this solution

[Edited on 15-2-2009 by Sedit]





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[*] posted on 15-2-2009 at 20:23


I would expect the green colour is from the nickel in the stainless reacting with the oxalic acid. Some yield is therefore likely to be compromised. http://physchem.ox.ac.uk/msds/NI/nickel_II_oxalate_dihydrate...
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[*] posted on 15-2-2009 at 22:09


Chances are your right, the color seems to fit and it dont appear that the steel is being heavyly corroded just discolored with a very fine sediment, after removel of the slight heat there is crystal formation so tommorow Ill be able to tell whats going on.

Always fun to know when you accidently create a cancer causing toxic substance:o





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[*] posted on 15-2-2009 at 23:46


Quote:
Originally posted by chemrox

I see two questions here. Yes Schiff bases are isolated all the time before the reduction is done. With ketones you need a catalyst like p-toluenesulfonic acid. A few crystals.

Are they isolated just like amines (ie. extract, acidify, risnse/repeat)?
Quote:

You're planning on an aluminum amalgam redux? You will have some washing up to do after that.

Actually, I was planning on exploring whether thiourea dioxide (http://www.sciencemadness.org/talk/viewthread.php?tid=11785) is suitable for performing the reduction, naturally I will need some sort of way of quantitatively measuring yield, so the reduction procedures detailed on Rhodium are unsuitable for research.

Formula409.

[Edited on 16-2-2009 by Formula409]
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[*] posted on 16-2-2009 at 00:34


As i know, the shiff base can be easily extracted by organic solvent. I've seen a procedure, where to P2P(probably, in some org solvent) was added some 25% ammonia solution, and this mixture was stirred to get a solution of P2P-imine in organic layer, which was further separated and reduced with NaBH4. Now i don't remember where i've seen it, but it seems to be a basic procedure for imines
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