tihkalmypihkal
Harmless
Posts: 2
Registered: 13-11-2012
Member Is Offline
Mood: No Mood
|
|
Need an ether replacement
So I came across this synthesis....
72.5g of aluminum foil is cut into one inch squares and placed into a 3000ml erlenmeyer flask or other suitable glass container. A solution of 1.8
grams of mercuric chloride (HgCl2) in 2530 ml water is added, and the mixture is stirred occasionally over 30 minutes to amalgamate the aluminum. The
solution is poured off and the foil is washed with four one-liter portions of water.
To the amalgam is added, in sequence, 80g of ammonium chloride in 101ml of water, 302ml of isopropyl alcohol (100%), 244ml of 25% NaOH solution, 89g
(0.5 moles) of piperonylacetone, and then 588ml of isopropyl alcohol. The mixture is swirled occasionally for two hours, and kept below 60°C by
cooling with an ice bath as necessary.
The mixture is then filtered through Celite (a diatomaceous silicate powder which is placed in a layer over the filter paper before filtering, it is
sold by chemical companies as Celite), and the filter cake is washed thoroughly with methanol. Combine the liquid filtrates and distill off the
methanol (65°C), isopropyl alcohol (82°C) and the water (100°C).
Dissolve the oil in 200ml of ether, and extract the MDA into two 500 ml portions of 3N HCl. The acid solution is washed with three portions of
methylene chloride equal in volume to the acid solution (you will probably have to wash portions of the solution at a time unless you have a huge
separatory funnel). The acid solution is basified with excess 25% sodium hydroxide solution (red litmus turns blue) and the liberated oil is extracted
into three 500ml portions of methylene chloride.
The methylene chloride solution is dried with magnesium sulfate. The drying agent is filtered out and the methylene chloride distilled out. The
residual oil is distilled under reduced pressure and the distilled oil then dissolved in ether
(or toluene or methylene chloride). HCl gas is bubbled through the solution until no more precipitate is formed. The precipitate is filtered off and
allowed to dry (~70% yield can be expected
I see that in the end ether can be replaced with toluene or DCM, my question is if it could be replaced in the first part as well? Also I was
wondering if MD P2P could be used in place of the piperonalacetone...I read somewhere that these two are interchangeable in synthesis?
[Edited on 14-11-2012 by tihkalmypihkal]
|
|
chemrox
International Hazard
![*](images/xpblue/star.gif) ![*](images/xpblue/star.gif) ![*](images/xpblue/star.gif) ![*](images/xpblue/star.gif)
Posts: 2961
Registered: 18-1-2007
Location: UTM
Member Is Offline
Mood: LaGrangian
|
|
This is pretty thoughtless. When you look at common names and chem slang figure out what the molecules look like. The reason we don't answer these
kinds of questions as a rule is not because we're all pious anti drug cops but because we want the discussions to be about chemistry not cookery.
In a new online forum its always a good idea to tread lightly until you have a feel for the ground. Some very smart people hang out here. Don't
underestimate this group.
"When you let the dumbasses vote you end up with populism followed by autocracy and getting back is a bitch." Plato (sort of)
|
|
tihkalmypihkal
Harmless
Posts: 2
Registered: 13-11-2012
Member Is Offline
Mood: No Mood
|
|
I didnt underestimate anyone, I am not a chemist, i am writing a paper on the subject of clandestine drug manufacture for a class and as ether seems
to be the only chemical in this reaction that is not easily obtainable, I was interested in commenting on it in my paper, but i need to know how it
could be accomplished by a clandestine cook. Based on my understanding, the
'3,4-Methylenedioxyphenylpropan-2-one" is the easiest precursor to make using the Wacker Oxidation with PdCl2. I asked here because this seemed like
a site where people would be able to answer this question. I am sorry, and I mean no harm but this is not a question that can just be googled, and I
dont have the time to learn chemistry before my paper is due. Just looking for some help from someone who knows. I have researched a lot and have
gained a good deal of chemistry knowledge, I actually plan to take an introductory course because of it, and maybe then I could contribute more to the
complex discussions on this site, but for now I'm not in that league. Sorry my ignorance offended you.
'
[Edited on 14-11-2012 by tihkalmypihkal]
|
|
watson.fawkes
International Hazard
![*](images/xpblue/star.gif) ![*](images/xpblue/star.gif) ![*](images/xpblue/star.gif) ![*](images/xpblue/star.gif)
Posts: 2793
Registered: 16-8-2008
Member Is Offline
Mood: No Mood
|
|
If you're going to quote something you found on the internet, then there
are two points of decorum to observe. (1) Provide a citation. Easy enough, I'd think. (2) Put it in inside BBcode quotation markup
[quote] ... [/quote]. There's a voice-bubble icon in this board's editor to assist with that.
|
|
Nicodem
Super Moderator
![*](images/xpblue/star.gif) ![*](images/xpblue/star.gif) ![*](images/xpblue/star.gif) ![*](images/xpblue/star.gif) ![*](images/xpblue/star.gif) ![*](images/xpblue/star.gif)
Posts: 4230
Registered: 28-12-2004
Member Is Offline
Mood: No Mood
|
|
You came across it WHERE? This is a science forum. Quoting without providing a reference does nothing but showing your disrespect
toward the scientific method.
Quote: | (~70% yield can be expected |
Of what? We have yet to see such yields of reductive amination of a ketone with NH3 by using aluminium amalgam. Where is the analytical
part of the experimental?
Quote: | I see that in the end ether can be replaced with toluene or DCM, my question is if it could be replaced in the first part as well?
|
Then you said: "I have researched a lot and have gained a good deal of chemistry knowledge". So you lie to us?
Quote: | Also I was wondering if MD P2P could be used in place of the piperonalacetone...I read somewhere that these two are interchangeable in synthesis?
|
What are you talking about? Interchangeable?
MDP2P is an acronym that drug cooks use for 1-(1,3-benzodioxol-5-yl)propan-2-one.
Quote: | I didnt underestimate anyone, I am not a chemist, i am writing a paper on the subject of clandestine drug manufacture for a class
|
What makes you feel that we would so readily eat shit from you? You just cold-bloodedly offended most of our members by underestimating our
intelligence and then you go up serving us more and more lies. If you are a clueless wannabe drug cook, at least have the decency to say so. It would
be better than treating us like idiots.
[Edited on 14/11/2012 by Nicodem]
…there is a human touch of the cultist “believer” in every theorist that he must struggle against as being
unworthy of the scientist. Some of the greatest men of science have publicly repudiated a theory which earlier they hotly defended. In this lies their
scientific temper, not in the scientific defense of the theory. - Weston La Barre (Ghost Dance, 1972)
Read the The ScienceMadness Guidelines!
|
|
woelen
Super Administrator
![*](images/xpblue/star.gif) ![*](images/xpblue/star.gif) ![*](images/xpblue/star.gif) ![*](images/xpblue/star.gif) ![*](images/xpblue/star.gif) ![*](images/xpblue/star.gif) ![*](images/xpblue/star.gif) ![*](images/xpblue/star.gif)
Posts: 7990
Registered: 20-8-2005
Location: Netherlands
Member Is Offline
Mood: interested
|
|
Drug cookery.
|
|
woelen
|
Thread Moved 14-11-2012 at 07:10 |
Nicodem
|
Thread Moved 14-11-2012 at 07:11 |
FishFloyd
Harmless
Posts: 1
Registered: 7-11-2012
Member Is Offline
Mood: No Mood
|
|
Hello; this is my first post here after lurking for a while, and whilst I realize that posting on an all-but-abandoned thread about drug cookery isn't
really the best debut one could make, I just wanted to state that the name "tihkalmypihkal" is the funniest thing I have read all day. ![:D](./images/smilies/biggrin.gif)
Cheers.
I have zero idea what I'm talking about one hundred percent of the time.
|
|
zed
International Hazard
![*](images/xpblue/star.gif) ![*](images/xpblue/star.gif) ![*](images/xpblue/star.gif) ![*](images/xpblue/star.gif)
Posts: 2281
Registered: 6-9-2008
Location: Great State of Jefferson, City of Portland
Member Is Offline
Mood: Semi-repentant Sith Lord
|
|
Substitution of solvents. Easy enough. I used to routinely substitute benzene or toluene for ether. Not in every case, but in many.
Ether is generally OK to work with, but it's touchy. It's low boiling, it likes to form explosive peroxides, and it is wildly flammable. Flicking a
light switch, at an inopportune moment, can cause your home to disappear. It is wise to know exactly what you are doing when working with ether.
Otherwise, you could end up a crispy critter.
|
|