Author Topic: iodosafrole writeup (Read 650 times)

jon · « **on:** November 11, 2009, 02:13:08 AM »

Jon we cool and all but your lack of trying is starting to piss me off so I will ask you to correct the highlighted areas because they are obvious and proof that the preview button was not even looked at before you posted this.
~SEDIT

ok
safrole was brominated with 1.9 moles per mole of HBr 40% in glacial acetic acid for 24 hours at 0 c 110 grams yeilded 144 grams bromocompound.
high yelids above 90 %
this was poured onto equimolar potassium iodide acetone was added (this is not critical ki is only sol 1g/100ml)
so maybe 150 ml acetone.
this was mixed and any clumps broken up for 30 minutes the precip is notably different in crystaline appearance.
the acetone oured off and the salts rinsed w acetone acetone evaporated iodosafrole has a much darker color than iodosafrole.iodosafrole is not darker then iodosafrole.... Pay attention.

8 gram molesGrams or moles?

MeNH2proper notation required to avoid confusion is bubbbled into dry iso heet to obtain 15% concentration.
this was mixed in sealed container.
stand 30 minutes.
vac evap methamine/alcohol (keeps
smell down) using aspirator equal water was added and ph adjusted to 12, and guess what fell out?
a gorgeous yellow oil from 110 grams
around 115 grams mdma base not salt was obtatinedsp.

Written by me Sedit

Jon..... You are getting sloppier and sloppier. I am no grammer nut or a prud for that matter but its as though you are not even your old self anymore and are just going around in an attempt to disrupt the current structure of things. If I am off base please PM me and explain the current situation but we have standards here and I would like to hear privatly why you are doing what ever you can to ignore them.

jon · « **Reply #1 on:** November 11, 2009, 05:39:02 AM »

you bees need to jump on this! and quit being all tedious.
better yeilds, and shit simple.
jon has a knack for locating chemical shortcuts.

zzhuchila_clocker · « **Reply #2 on:** November 11, 2009, 07:38:57 PM »

thanks, jon! the only question is the presence of bis(2- 3,4-methylenedioxyphenyl-isopropyl)-N-methylamine, obviously it is difficult to get rid of it(maybe by salt crystallization), but if you used excess of 8 moles of MeNH2, its content should be low. Anyway if it is not toxic, then its fine. Is that 115g of freebse MDMA after acid-base extraction purification. Imean there could be some unreacted halocompound or safrole resulted from elimination otherwise

jon · « **Reply #3 on:** November 11, 2009, 08:02:45 PM »

trust me with that stochiometry there are scant by-products as explained the excess supresses side rxns swij has eaten hundreds of grams of this stuff and he's still kicking.

115 grams base around 200 grams acetate salt

vajrakana · « **Reply #4 on:** November 12, 2009, 05:23:38 AM »

So, the Ki swaps and you get KBr. Where does that go?

The iodine is substituted and you get methyl iodide, yes? That has a BP of 43C or so, and acetones is around 56C, so yes, you could get the MeI off with vacuum, along with everything else, but I'd still want to further process the base to get it more pure.

This process should work with methyl eugenol as well, as a test substrate.

Sedit · « **Reply #5 on:** November 12, 2009, 06:16:52 AM »

The KI undergoes a Finkelstein reaction with a Bromoalkane in acetone to yeild the much better leaving grouping of Iodoalkane and KBr.

This should hold true for the reactions stated using MeBr and NaI like you discussed to yeild MeI but that is a mute point at the moment I believe.

@zz-zhuchila
The general rule is to keep a 10x molar excess of the amine to the haloalkane to prevent the side reactions in discussion. In the old days when safrole was at the local hippy shop this proved a pain in the ass on 100 gram batches but for small scale synthesis it proves much less of a problem when considering risk(waste) vs reward factors.

@Jon aside from my critique of your posting style I thank you much for your sharing of the information gathered thru experimentation.

~Sedit

jon · « **Reply #6 on:** November 12, 2009, 09:26:14 AM »

you can scale that ad infinitum no probs 8 moles works fine the books say 10 but expiriment is king.
amen brothers that concludes todays sermon, now let us pray.

p.s.

This process should work with methyl eugenol as well, as a test substrate

of course it would.
it''s been used to synth dmmda-2 in 90% yeilds
mmda too. very versatile.
let's start bubblin folks
can you say amphetamine buffett?
all 10 essential amphetamines being served tonight.
yeah!!!

Wizard X · « **Reply #7 on:** November 12, 2009, 10:35:29 AM »

My advice is react safrole with 40%+ HI [1] @ 0-1 oC for 24 hours. Hydriodic acid can be made via sodium (or potassium) iodide with 1 M phosphoric acid solution and then azeotropic distillation.

Bubble dry methylamine gas into 0-1 oC dry isopropanol.

[1] http://en.wikipedia.org/wiki/Hydrogen_iodide & http://designer-drugs.com/pte/12.162.180.114/dcd/chemistry/hydriodic.argox.html

Some trivia: hydriodic acid in an aqueous solution as an aphrodisiac to heighten sexual desire, US Patent 5281423, http://www.freepatentsonline.com/5281423.html

jon · « **Reply #8 on:** November 12, 2009, 11:29:23 AM »

what genius! mr wizard, they don't call mr smarty for nothin, what a badass!
i prefer to avoid spliting methyene dioxy ethers so i don't fool woth hi besides this is easy.

in regards to:
Written by me Sedit

Jon..... You are getting sloppier and sloppier. I am no grammer nut or a prud for that matter but its as though you are not even your old self anymore and are just going around in an attempt to disrupt the current structure of things. If I am off base please PM me and explain the current situation but we have standards here and I would like to hear privatly why you are doing what ever you can to ignore them.

that'a my writting style when i'm on ecstacy sorry, i'll take some composition classes and try to pay attention in class next time.

awww shucks it's the other way around the stochiometry is 1.9 moles hbr per mole of safrole, hopefully anybody with common sense would know safrole is a *very* limiting reagent if ya catch my drift.

Wizard X · « **Reply #9 on:** November 12, 2009, 09:20:17 PM »

Quote from: jon on November 12, 2009, 11:29:23 AM

what genius! mr wizard, they don't call mr smarty for nothin, what a badass!
i prefer to avoid spliting methyene dioxy ethers so i don't fool woth hi besides this is easy.

Both HBr and HI WILL cleave ethers AT 100 oC (or reflux), BUT NOT at 0-1 oC.

jon · « **Reply #10 on:** November 13, 2009, 12:57:53 AM »

no shit but does;nt hi have to be superconcentrated to add to the alkene???
you mentioned 40%

Wizard X · « **Reply #11 on:** November 13, 2009, 01:27:27 AM »

Quote from: jon on November 13, 2009, 12:57:53 AM

no shit but does;nt hi have to be superconcentrated to add to the alkene???
you mentioned 40%

No! 38% HBr will add to the alkene. The more concentrated the HBr, or HI, is the less reaction time is need at 0-1 oC. 38% w/w acid, and higher will work.
Try a micro-experiment of safrole (or eugenol) with 38% w/w HBr and 38% w/w HI @ 0-1 oC for 24 hours.

Cleavage of acyclic ethers. http://en.wikibooks.org/wiki/Organic_Chemistry/Ethers

Acyclic ethers can be cleaved by a strong acid, typically HI or HBr, but not HCl. The acid breaks the ether apart into an alcohol and an alkyl halide (a haloalkane.) Cleavage of ethers by an acid was first seen by Alexander Butlerov in 1861, when he discovered that hydroiodic acid causes 2-ethoxypropanoic acid to break apart into iodoethane (ethyl iodide) and lactic acid (2-hydroxypropanoic acid.) The mechanism used in acidic cleavage of ethers depends on whether they have primary, secondary, or tertiary groups attached to oxygen. If one of the carbons attached to the central oxygen atom is tertiary, benzylic (contains benzene ring), or allylic (contains carbon-carbon double bond), then the cleavage will occur via an SN1 or an E1 mechanism. The E1 mechanism leads to an alcohol and an alkene instead of an alkyl halide. These reactions often take place around 0 degrees C. On the other hand, if both groups attached to the central oxygen atom are primary or secondary, the reaction takes place via an SN2 mechanism. These reactions are often conducted at 100 degrees C.

jon · « **Reply #12 on:** November 13, 2009, 01:49:41 AM »

very informative!!!
iodides are sort of watched and it's much easier my way because hbr can be made by just adding h2so4 to nabr in acetic acid.
and the rxn goes complete because it's so dry.
yeilds are very high.

Vanadium · « **Reply #13 on:** November 17, 2009, 01:21:22 PM »

Quote from: jon on November 12, 2009, 09:26:14 AM

you can scale that ad infinitum no probs 8 moles works fine the books say 10 but expiriment is king.
amen brothers that concludes todays sermon, now let us pray.

p.s.

This process should work with methyl eugenol as well, as a test substrate

of course it would.
it''s been used to synth dmmda-2 in 90% yeilds
mmda too. very versatile.
let's start bubblin folks
can you say amphetamine buffett?
all 10 essential amphetamines being served tonight.
yeah!!!

Jon you only point out methoxylated phenylpropenoids and allylbenzenes as substrates, is this coincidence or is there a specific reason for this? Why strictly methyl eugenol and not eugenol or desmethyl eugenol?

jon · « **Reply #14 on:** November 17, 2009, 07:18:54 PM »

in the other thred i suggested the hx could be aded cool to the alken then heated to split off the alky aryl ether then the williamson ether synth ether synth with KF and diiodomethane.
dibromo no work gottaa be diodo.
only question would that base cause e1,e2 side rxns???
if not then you could go straight to mdma in 90 % yeilds.

rvd · « **Reply #15 on:** November 19, 2009, 09:33:32 PM »

hey cheers for this info jon, tis quite interesting. Just wondering if swapping MeNH2 for NH2 would work to form mda instead?

Wizard X · « **Reply #16 on:** November 19, 2009, 10:23:34 PM »

Quote from: rvd on November 19, 2009, 09:33:32 PM

hey cheers for this info jon, tis quite interesting. Just wondering if swapping MeNH2 for NH2 would work to form mda instead?

Yes!

jon · « **Reply #17 on:** November 20, 2009, 07:29:34 AM »

methylamine at 20% conc. reacts in less than 15 minutes at 90 + yeilds personal experience you base it and a golden yellow oil falls out that simple.
it' mo betta man!!! try it pm me for pointers i'm here to help.
nh3 same damn deal rxn is a little slower use ipa the protons are sheilded and don't hinder the sn2 at all it goes it's concentration and water free dependant that simple bubbling is the real secret to getting this to work, it's a fucking art.

no1uno · « **Reply #18 on:** November 21, 2009, 09:51:35 AM »

Wonder what you'd get if you added 1-bromo-2-chloroethane to eugenol to form the furanyl ring then did this? That should give a 3-MeO-4,5-Furanyl-whatever shouldn't it?

jon · « **Reply #19 on:** November 21, 2009, 11:30:37 AM »

you have a knack for comming up with ideas that are inquisitive but have little scientific basis in fact show me the refs we'll talk about the "fly" cmpds.

Author Topic: iodosafrole writeup (Read 650 times)

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