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

fresh1

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Re: Short Question Thread 2.0
« Reply #80 on: June 09, 2012, 11:22:46 AM »

      MDP2P from safrole using H2SO4 and NH4NO3  :-\

    I havent seen this method here...fresh hasn't done this but is very interested in any wasps who have, it sounds interesting. :D

       any references to anything from anyone?  :)
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carl_nnabis

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Re: Short Question Thread 2.0
« Reply #81 on: June 10, 2012, 10:24:40 AM »
Oh off course it is also possible the other way round but it seems really impractical to me with reagents that are pretty hard to get... like butyllithium the most pyrophoric substance known to me...
wouldtn use it, even if you can get your hands on some what i really doubt because of shipping problems etc...
anyway heres a reference
hxxp://www.erowid.org/archive/rhodium/chemistry/isosafrole.piperonal.html
I think it can bee applied for any other benzaldehyde as well. But... are those aldehydes really more acquirable where you live? Its way more easy here to get these propenyl/allylbenzenes, just fractionate some essentials?
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lugh

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Re: Short Question Thread 2.0
« Reply #82 on: June 10, 2012, 07:54:29 PM »
Quote
MDP2P from safrole using H2SO4 and NH4NO3

That's a good way to ruin valuable safrole as while it's possible to form mdp2pol using published techniques such as those posted by drone 342, no one besides the original poster tBOC claimed success  ;) Simply speaking, it's yet more drivel from a troll ::)

Quote
Does anybody know any OTC qualitative test for Hg vapor in air beside CuI paper?

As far as mercury vapor detection, the attached article and patents may be helpful  8)
« Last Edit: June 10, 2012, 08:17:52 PM by lugh »
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fresh1

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Re: Short Question Thread 2.0
« Reply #83 on: June 11, 2012, 12:20:57 PM »
Quote
Simply speaking, it's yet more drivel from a troll ::)

thanx lugh, that's all I need to hear about it ... fresh feels very priviledged to have access to such experience as yours  8)

it didn't look right and I figured many must have trod this path before fresh and 'if' it worked surely it would have been discussed more :-\

fortunately fresh has a nest full of clever fellow wasps to help him avoid the fruitless searches and pointless experiments such bullshit may encourage :D 8)

thanx again ;)
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RoidRage

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Re: Short Question Thread 2.0
« Reply #84 on: June 16, 2012, 07:13:05 PM »
For those with experience with this reaction....When reducing a ketoxime with Al/Hg under acidic conditions ala Antibody,is there a dramatic drop in yield when substituting glacial acetic acid for concentrated hydrochloric acid or is it minimal ? It's mentioned in Antibody's write-up that HOAc give the best results but it's not clear whether or not it's vastly superior. GAA has been used with great success in the past but it's unfortunately not available in the moment. Preparing it from available chemicals (vinegar) seems tedious but will be done if using HCl really kill the yield...

carl_nnabis

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Re: Short Question Thread 2.0
« Reply #85 on: June 16, 2012, 09:14:48 PM »
somebody should not try it out with HCl it will definitely kill the yield!
maybe the GAA can be substituted with concentrated formic acid but I doubt really anything else will do...
but especially GAA has a buffer effect that should be considered  ;)
BUT! i have no practical experience i just know that an al/hg for nitrogroups can only be run usig acetic or formic acid!
« Last Edit: June 16, 2012, 09:16:20 PM by carl_nnabis »
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fresh1

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Re: Short Question Thread 2.0
« Reply #86 on: June 17, 2012, 03:40:25 AM »
what could be the worst that could happen if you ran it unbuffered?

 Could someone please explain the rationale behind buffering this synth :D
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atara

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Re: Short Question Thread 2.0
« Reply #87 on: June 17, 2012, 04:46:30 AM »
HCl is not HCl, it's HCl . H2O which is no good for amalgam reductions. You want dry acid, hence GAA. H2O will allow the nitro group to deprotonate and hydrolyse giving an alcohol... ethereal HCl works, but you don't have that.

edit: ethereal HCl does not work, disregard that
« Last Edit: June 19, 2012, 04:03:27 AM by atara »

fresh1

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Re: Short Question Thread 2.0
« Reply #88 on: June 19, 2012, 03:00:12 AM »
Formic acid would be the most comparable polar protic solvent to GAA

Again could someone explain to me what could/would happen running this rxn UNbuffered?

  IIRC  that was how it was 'originally done'  wasn't it
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atara

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Re: Short Question Thread 2.0
« Reply #89 on: June 19, 2012, 04:02:17 AM »
The Beckmann rearrangement can occur instead of reduction, giving PAA and methylamine.
« Last Edit: June 19, 2012, 04:04:20 AM by atara »

spice

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Re: Short Question Thread 2.0
« Reply #90 on: June 20, 2012, 10:56:31 AM »
dont know why vesp and sedit tolerate rats on this board...... >:(

lugh

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Re: Short Question Thread 2.0
« Reply #91 on: June 21, 2012, 06:20:16 PM »
Quote
dont know why vesp and sedit tolerate rats on this board.

Acids are protic by definition  :)  Our counselor has already proposed a solution to that issue  8)
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Sydenhams chorea

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Re: Short Question Thread 2.0
« Reply #92 on: June 21, 2012, 09:35:01 PM »
When a bleach product contains 33° chlorine, what is the % of NaOCl ?
It is perhaps the narcotic. Hyoscine affects certain people very oddly. One cannot be sure. Sometimes, these cases take strange forms. The victim becomes in a sense, 'mediumistic', a vehicle for all the intangible forces in operation around her.

Wizard X

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Re: Short Question Thread 2.0
« Reply #93 on: June 22, 2012, 03:46:44 AM »
When a bleach product contains 33° chlorine, what is the % of NaOCl ?

Read this: http://www.powellfab.com/technical_information/files/810.pdf
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Enkidu

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Re: Short Question Thread 2.0
« Reply #94 on: June 22, 2012, 07:32:45 AM »
Acids are protic by definition

I didn't read the thread, but on a pedantic note, so-called "Lewis acids" are electron acceptors. Really, donating a proton and accepting electrons are the same things..

Electro´S

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Re: Short Question Thread 2.0
« Reply #95 on: June 30, 2012, 10:23:15 PM »
Hi mates!!!
Thinking about the Strike route to oxime from Nitropropene using Tin Cl2·2H2O in Ethyl Acetate i fall in doubt when for the basification of the product he calls for Hydrogen Carbonate. Can anyone uses NaOH instead the weak HCO3? or  the strong NaOH would destroy the OXIME before extract it with the solvent? ???

Any other route "vol. effective" to the oxime will be appreciate.  :)

Thanks!!!

carl_nnabis

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Re: Short Question Thread 2.0
« Reply #96 on: July 09, 2012, 06:38:49 PM »
is it possible that  1 liter dcm in a glassbottle send in a parcel may combust because of the temperature outside?
edit: ive read in a translation engine combust actually has something to with flames and stuff, i just mean that the bottle will crack because of overpressure, its outside for sure at least high enough for DCM to boil if the bottle would ever get full sun exposition...
im just worried because it should have arrived yet, the postman even let a message here few days ago.....
« Last Edit: July 09, 2012, 07:51:33 PM by carl_nnabis »
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lugh

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Re: Short Question Thread 2.0
« Reply #97 on: July 09, 2012, 11:39:27 PM »
Quote
is it possible that  1 liter dcm in a glassbottle send in a parcel may combust because of the temperature outside?
edit: ive read in a translation engine combust actually has something to with flames and stuff, i just mean that the bottle will crack because of overpressure, its outside for sure at least high enough for DCM to boil if the bottle would ever get full sun exposition...
im just worried because it should have arrived yet, the postman even let a message here few days ago.....

DCM is nonflammable, but you apparently are unaware of recently published European Union regulations :

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

http://de.wikipedia.org/wiki/Dichlormethan

which are explained in the attached document  8)
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carl_nnabis

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Re: Short Question Thread 2.0
« Reply #98 on: July 10, 2012, 12:09:00 AM »
damned i knew its unflammable but its so low boiling it could crack the bottle... it didnt knew about the actual shipping laws, but on the other hand my chemical supplier is known to not work after actual shipping laws because he sends GAA for example which is forbidden, you have to get it personally if you need it ;D
fuck, i hope it has not cracked, because there sodium in the same parcel im readily fucked if it did...
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metamorphin

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Re: Short Question Thread 2.0
« Reply #99 on: July 10, 2012, 02:11:14 PM »
I don´t think it would crack, glass bottles can hold quite a lot of pressure, I once had a glass bottle with gasoline laying in my car for half a day and the temp inside was nearly 50°, I would estimate. Even though DCM boils much lower, I think you´re safe.

Also, the temperature in the parcel will most likely not exceed 20°C, even if it´s 30° or more outside, assuming it isn´t placed in the direct sunlight for an hour or so.

Good luck :)