Author Topic: Short Questions Thread  (Read 10820 times)

Vesp

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Re: Short Questions Thread
« Reply #360 on: January 05, 2010, 01:36:03 AM »
Also some reactions when left to sit may not need to be refluxed - I.e when producing methoxyphenol from hydroquinone, methanol, and sulfuric acid - you can either leave it for several days to stir, or reflux it only for a few hours.
So I have heard, this isn't from experience.
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shroomedalice

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Re: Short Questions Thread
« Reply #361 on: January 05, 2010, 01:42:52 AM »
bang on vesp :)

its all got to do with kenetic energy the more heat you put into the reaction the quicker it goes.

that does not mean they will not work if left to there own devices well some reaction anyway.

the same goes for the PAN to PAA though it will take you a month or so for the conversion to take place.

PAN to amide will take over night.

Sedit

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Re: Short Questions Thread
« Reply #362 on: January 05, 2010, 01:52:15 AM »
Many times its a function of the activation energy needed to overcome the initial equilibrium of the reaction. Once the needed energy is inputted it can be run higher or at a nice slow pace as long as this is sufficiant. The general rule is that a 50% increase in temperature in degrees C leads to a 100% increase in kinetic rate. So a reaction run twice as hot will run 4x faster.
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Sedit

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Re: Short Questions Thread
« Reply #363 on: January 05, 2010, 01:53:59 AM »
If something needs to reflux for a relatively long time, like 20 hours, can this be done cumulatively (ie. 10 hours one day and 10 the next) so it doesn't have to be left running overnight?


Yes. as said as long as its at the required temperature.
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timecube

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Re: Short Questions Thread
« Reply #364 on: January 06, 2010, 05:14:16 PM »
Thanks for all the info, guys.  ;D

If I had a place to keep all this stuff, I'd be up and running in a week.  It sucks living with other people who wouldn't understand.  :-\

Naf1

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Re: Short Questions Thread
« Reply #365 on: January 07, 2010, 12:58:52 AM »
Hey Tim, put a timer on your pump for you condenser and hotplate! Set it for 20 hours and cover it up, and then go and act as if you are not conducting a 20 hour reflux! As you dont need to sit there and watch it for 20 hours, when you are at reflux everything is going smoothly you can go and do other things (like sleep, watch TV etc), best bet is to keep the condenser running and just have the timer turn the hotplate off after 20 hours. Go to bed and in the morning go and stop the pump and youre done!!!

shroomedalice

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Re: Short Questions Thread
« Reply #366 on: January 07, 2010, 01:31:12 AM »
BANG  house starts to fill with acrid smoke and you wake to find that you can not breath or see.

the fire alarm in the lab wont work as its been eaten by the acid vapor in seconds and a small fire has
started in the lab.

you try and walk to your door but keep on hitting the wall as you can not see or breath.
the fire is getting more intense and you are starting to pass out as you still can not breath.

this is a scene from a possible fucked up loomins that realy needs 16 hours to compleate some times even over 24.

not all reactions go like this if they screw up but just a warning be damb carefull what you decide to sleep through.

Naf1

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Re: Short Questions Thread
« Reply #367 on: January 07, 2010, 01:47:32 AM »
Worse thing that has happened to me in many years of work, is the bottom condenser hose somehow comes off. Which effectively stops refluxing and whatever you were refluxing starts filling the air, and water goes literally everywhere as the pump just keeps pumping. I have preformed countless 48hour reflux's with hydroiodic acid, also many I just leave to reflux overnight if it is longer than 5 hours. Are you proposing to watch it for 20 hours? As even if I have a 5 hour reflux I will get it to reflux then leave, and come back in about 5 hours, sometimes I check on it while its refluxing but rarely.

shroomedalice

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Re: Short Questions Thread
« Reply #368 on: January 07, 2010, 01:52:19 AM »
and I would belive it to naf thats about the worst most people will encounter but some reactions are truly cunts
and thats all there is too it.

we may have main routes we all follow but there will be a few that read all of this one day and they will end up with the
cunt reaction :).


Bluebottle

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Re: Short Questions Thread
« Reply #369 on: January 19, 2010, 12:29:15 AM »
I'm not entirely sure of the solubility of potassium borate in trimethyl borate/methyl iodide/acetone, but I don't think it's all that much. So wouldn't it be possible to get methyl iodide from trimethyl borate added to a solution of KI in acetone?
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2bfrank

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Re: Short Questions Thread
« Reply #370 on: January 22, 2010, 10:49:48 PM »
I haven't seen much info, nor being able to google it, on a nitroaldol henry type reaction between benzaldehyde and 2-nitroethylbenzene, yielding 1,3 diarylnitropropene. This product could be converted to a 1,3 diaryl-2-propylamine or converted to a ketone and then with a reductive animation converted to a 1,3,diaryl,n-methyl-2 propylamine. Sorry if my nomenaclature is bad, but I am surprised that their is little found, well at least for me. I stumbled upon some of these reactions in a thesis, but only to the point of the 1,3 diarylnitropropene. If anything, I wouldn't be surprised if such molecules were inhibitive of the enzymes, related to the pathway associated with the use of amphetamine type structures, but thats a guess and may be wrong. I did notice in Java's article of interest thread,
http://127.0.0.1/talk/index.php/topic,568.msg7202.html#msg7202  that diaryl molecules were mentioned, and seeing this triggered my thoughts on what I have presented. I dare say experimental is king. I just wanted to mention it I suppose. My question is, has anyone heard or seen such a molecule being discussed or prepared etc. I haven’t checked other forums, etc.

Enkidu

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Re: Short Questions Thread
« Reply #371 on: January 22, 2010, 11:14:31 PM »
You're basically talking about a compound that's very structurally close to lefetamine, the only differences being that it's a secondary amine instead of a tertiary and there is an appropriately placed methylene spacer between one of the aryl groups and the main carbon chain? Check out desoxypipradrol type stimulants, that's where the gold is if you want to use a couple of phenyl moieties.

Those 1-phenethylamines are useless, btw. I can't comment conclusively on your proposed molecule, but i doubt that it will be an active stimulant or entheogen.

2bfrank

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Re: Short Questions Thread
« Reply #372 on: January 23, 2010, 02:37:10 AM »
Thanks Enkidu for your comments, and I will certainly look up that molecule that is a tertiary amine. Im still surprised to find little on what Ive presented, albeit a likely - no contender. Perhaps I am not looking hard enough, or in the correct places. Still interesting but/.

« Last Edit: January 23, 2010, 03:50:47 AM by 2bfrank »

2bfrank

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Re: Short Questions Thread
« Reply #373 on: January 23, 2010, 09:30:00 AM »
Anyone got a ref, or info on this.."oxidation of naphthalene in concentrated sulphuric acid in the presence of mercury sulphate" to yield phthallic anhydride.

Vesp

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2-Hydroxy-6-MethylBenzaldehyde
« Reply #374 on: January 28, 2010, 02:59:22 AM »
Does 2-Hydroxy-6-methyl-Benzaldehyde have any interesting uses?
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Sedit

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Re: Short Questions Thread
« Reply #375 on: January 28, 2010, 04:47:33 AM »
It sounds simular to a substance you can put in a discrete package and send to Sedits nationwide. Just a hunch though  ;D


LOL lemme stop wasting your time here. Other then the OH methylated variety turned amphetamine I can't think of many uses off the top of my head.
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Enkidu

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Re: Short Questions Thread
« Reply #376 on: January 28, 2010, 06:50:21 AM »
haha, well, oxidation with permanganate and dehydration to the anhydride. Maybe you could use it as a protecting group if you turned the phenolic ~OH into an ether.

timecube

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Re: Short Questions Thread
« Reply #377 on: January 29, 2010, 11:11:49 AM »
It's my understanding that acidified MeOH can be used in place of DMS in many instances, and using higher ratios of sulfuric acid/MeOH gives better results.

http://www.springerlink.com/content/7072587ll242u23l/
http://www3.interscience.wiley.com/journal/113320198/abstract


My question is how do you calculate the right stoichiometric amounts to use in place of a certain amount of DMS?  Since distilling acid/MeOH to dryness yields DMS, my assumption would be that acidified MeOH just acts to form DMS dissolved in MeOH in situ, and since DMS only gives up one of it's methyl groups, you need at least twice the molar ratio of MeOH to the amount of DMS that was originally required.  Is this right, close, way off?

In the first paper I linked, they seem to just be trying a slew of ratios to see which one works best.

shroomedalice

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Re: Short Questions Thread
« Reply #378 on: January 29, 2010, 03:33:16 PM »
I dont think you will have much luck with just acid and methanol.

still I could be wrong but I think if it worked SM would be all over it.

Enkidu

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Re: Short Questions Thread
« Reply #379 on: January 29, 2010, 06:41:06 PM »
Why not? Oxalic acid may have some special properties, but when you get down to it it's just a fisher esterification. Which thread discusses this at SM?