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Author Topic: Jon's route  (Read 3445 times)

igotthere

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Re: Jon's route
« Reply #40 on: July 23, 2012, 10:02:29 PM »
Fuck. I used IPA not acetone.
What was I thinking... So do you think I have fucked the bromo? should I just start again?
Jon I need help! I'm running out of time, my dry Ice arrives tomorrow and realistically I only have wed, thursday and friday evening to myself before I put a lid on my chem for a while.

Thx for noticing polonium.. what an idiot :(

igt

igotthere

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Re: Jon's route
« Reply #41 on: July 23, 2012, 10:17:14 PM »
how embarrassing that I thought I saw purple tinges too... now when I look I can't really see it at all.
Was a definite purple colour on the kitchen roll I used to clean the flask though?

bubble

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Re: Jon's route
« Reply #42 on: July 23, 2012, 11:01:15 PM »
if you use IPA instead of acetone not all of your KI will get KBr because the use of acetone puts the balance to the non soluble KBr. So KBr is not really soluble in IPA so a lot will precipitate, but not all because KBr is non soluble in acetone and slightly soluble in IPA. I think some of the KI didn't switched to KBr. So I think you have a mixture of bromosafrole and iodosafrole. You can extract the whole thing out of your IPA if you did it you can dissolve it in some acetone and add again some KI. After this you can easily extract your nearly clean iodosafrole and some KBr should precipitate. This would save you a lot of work and you don't have to start from the beginning.

lugh

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Re: Jon's route
« Reply #43 on: July 23, 2012, 11:43:31 PM »
As mentioned in:

http://127.0.0.1/talk/index.php/topic,828.0/all.html

a series of unfortunate events led to the posting of the thread on the Hive in which this reaction was discussed at in detail  ;) There are many other threads on this website and others in which the halo routes are discussed:

http://127.0.0.1/talk/index.php/topic,1833.0/all.html

http://127.0.0.1/talk/index.php/topic,1697.0.html

http://127.0.0.1/talk/index.php/topic,1246.0/all.html

http://127.0.0.1/talk/index.php/topic,828.0/all.html

and

https://the-collective.ws/forum/index.php?topic=22523.0;all

https://the-collective.ws/forum/index.php?topic=23099.msg161953#msg161953

As far as the Finkelstein reaction:

Dipolar Aprotic Solvents in Bimolecular Aromatic Nucleophilic Substitution Reactions

J. Miller, Alan J. Parker
J. Am. Chem. Soc., 1961, 83 (1), pp 117–123
DOI: 10.1021/ja01462a023
Publication Date: January 1961

and

THE REACTION OF PROPENYLPHENOL ETHER DIBROMIDES WITH SODIUM IODIDE

J. KOVÁCS
J. Org. Chem., 1950, 15 (1), pp 15–18
DOI: 10.1021/jo01147a003
Publication Date: January 1950

are attached  8)

« Last Edit: July 24, 2012, 12:02:43 AM by lugh »
Chemistry is our Covalent Bond

Polonium

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Re: Jon's route
« Reply #44 on: July 24, 2012, 01:39:35 PM »
Don't worry all is not lost. These things happen. bubble has it spot on. The Finkelstein is driven forward by the insolubility of KBr in acetone. Just checked there and it appears that KBr is only soluble at 1g/100ml in ethanol. It should be someone similar in IPA. Most of you bromosafrole should be converted to the iodo already. To be sure you can always just perform the reaction again in acetone and work it up. You can probably use a bit less KI too as there is sure to be some bromosafrole converted already.

Best of luck with your dreams igotthere. BTW have you got molecular sieves for drying the IPA or how do you plan on gassing? Might be good to split it in two batches in case there is too much water in the IPA/amine solution. If your stuck you can instead perform an SN2 amination in DCM (Here is a ref: http://127.0.0.1/talk/index.php/topic,1833.msg31231.html#msg31231)

I hope you get there!

igotthere

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Re: Jon's route
« Reply #45 on: July 24, 2012, 06:30:47 PM »
thanks for replies.

Bubble: I'd already evap'd off my ipa and had what I 'thought' was idosaf in a jar in the fridge.
So I did what you suggested and took the oil, dropped in 1.1 moles ki and spun for 40mins. Didn't really notice any colour change this time.
I stoppered the flask and am just evapping off DCM (hairdryer on side of jar... bad technique? is only 40ml?)

the colour doesn't really look like dark black/purple if I'm honest, but there is still lots of  dcm in there so I'll report back on that.

Lugh: thanks very much for doing what I should have done and utfse... I do appreciate your help.

Polonium: Thanks for your words of encouragement! I have 3a sieves that I plan on using in situ in my IPA after Fractal reported prbs on his first attempts. I'll also build some sort of drying tube packed with mgso4.
I have dry ice and methylamine hcl waiting in the wings.
I also brominated another 20ml of safrole this morning (8am) so I'll make sure I don't use IPA on this batch... 

My gassing rig is pretty much ala jons ghetto gass generator (gatorade/enema bottles) albeit on a much smaller scale.
I've used 250ml plastic drink bottles. I have 4mm id clear plastic tubing running from the first bottle to the second bottle.
I've push the tube into the first bottle only a couple of inches. I've then run the other end into the second bottle (suck back trap) and again have only inserted this end a couple of inches.
I have then taken a second tube and inserted it all the way down to the bottom of the second bottle, then out and into my metal vessel that will hold the dry chilled IPA (my metal vessel is an aluminium drinks can with the lid off. ok to use?)
As a precaution against leaks and bottles tipping over I have silicone sealed the tubes on the inside and outside of the lids and I have cut some sheet lead squares and siliconed the bottles to them. This works a treat and keeps them nicely upright.

A couple of questions: is my aluminium drinks can ok to use as a IPA vessel?
Also when evaporating off dcm with a hairdryer the temp directly in front of the glass jar is around 80deg c. Is this liable to cause decomposition of the idosafrole or is is a safe temp?

edit: hmmm the idosaf doesn't seem to have any purple colour at all, although it is much much darker this time round. is very dark browny colour that, when swirled, has a kind of toffee/golden colour when swirled up the side of the jar.


thanks

igt
« Last Edit: July 24, 2012, 06:46:12 PM by igotthere »

igotthere

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Re: Jon's route
« Reply #46 on: July 25, 2012, 04:09:27 PM »
can anyone help with my questions? I'm good to go tonight so would really appreciate some feedback regarding the use of aluminum can as a vessel to catch my methylamine.

also the temp that decomposition of idosaf occurs at would be good too please. igt

bubble

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Re: Jon's route
« Reply #47 on: July 25, 2012, 04:33:27 PM »
hey igotthere,
I wouldn't recommend the use of an aluminium can or vessel because aluminium is really non noble and so it can corrode.

The story with the hair dryer i think you don't need to get nervous because the solution only get the temperature of the boiling point of the solving agent which in this case is DCM with a b.p. of 39,7°C. So don't make you nervous. If the amount of solving agent is getting lower, just hold your hairdryer a bit more away.

igotthere

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Re: Jon's route
« Reply #48 on: July 25, 2012, 05:53:59 PM »
thx bubble for yr quick response

igotthere

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Re: Jon's route
« Reply #49 on: July 26, 2012, 10:11:37 PM »
So I gassed my IPA.
I had my first idosafrole which was the one I fucked up by adding IPA rather than acetone, plus a second batch.

I gassed both of them. They are both now sitting in jars, both yellow, one yellower than the other.

I'm going to be honest now..
I don't know what to do next.

I think I've read that Jon has ph'd to 12, evapped everything off and just eaten raw mdma freebase?!
I'd rather get hcl.

Could someone give me a pointer?

igt

bubble

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Re: Jon's route
« Reply #50 on: July 26, 2012, 11:16:22 PM »
wait till morning... or wait some hours xD i don't know where you are from. Here it's nearly 1 in the morning. Then make it basic to ph 12 and extract with some DCM or ether. Dry the DCM with some anhydrous Na2SO4 for 12 hours to get all of the water out of it and then bubble HCl gas through it. This will precipitate the hydrochloride salt. Filter it off and if you want to get it very pure which should be nearly but if you want to purify it to the maximum, basify it in a solution, wash with DCM or ether again, dry it with Na2SO4 which was made anhydrous. And again bubble some really dry HCl gas through it. Now really white powder should precipitate which can be solved in some hot water to make a hot saturated solution which is then slowly (really slowly, i would recommend a sand bath) cooled down to get some big chrystals.

igotthere

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Re: Jon's route
« Reply #51 on: July 28, 2012, 02:38:38 PM »
Thx Bubble.
I'm assuming I bring the ph down with hcl?
also, I have mgso4 and 3a sieves, would any of these be sufficient?

igt

igotthere

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Re: Jon's route
« Reply #52 on: July 28, 2012, 03:27:14 PM »
hmm I just tested my two jars, the first one measured ph 11.2 the second one ph 9.8

So it seem that I need something alkaline to get to ph 12? if so what would I use, or are they both ok as they are below 12?

thanks and sorry for silly questions - i really don't know what I'm doing..

igt

bubble

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Re: Jon's route
« Reply #53 on: July 28, 2012, 08:25:11 PM »
you can bring the pH with some NaOH or KOH to the pH of 12... 11.2 will also be enough. The high pH is to form the free base of your mdma which is soluble in ether or DCM but not in water. The HCl gas is to get the mdma-hydrochloride which is soluble in water but not in your unpolar DCM/Ether. This is a simple acid-base extraction which will push the purity of your mdma to really good stuff. Bubble only HCl as long in there as something precipitate. If nothing precipitate it's enough.

I've heard that MgSO4 is not the best drying agent for amines. The 3A sieves should go but it's way easier to use some Na2SO4 which is pH neutral and is really good to dry that shit out of it.

igotthere

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Re: Jon's route
« Reply #54 on: July 28, 2012, 11:50:44 PM »
thx bubble, is bedtime over here now but I should have some time tomorrow to push things along.

igt

T-cowboy

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Re: Jon's route
« Reply #55 on: July 30, 2012, 10:53:01 AM »
Just evap the IPA first.. But i guess you have done something else.. oh and gassing HCl into mdma freebase can be a real pain in the butt..

Where in the process are you now?

igotthere

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Re: Jon's route
« Reply #56 on: July 30, 2012, 08:36:20 PM »
T Cowboy, are you suggesting evapping the IPA and then altering PH?
Am still at the stage I was at a few posts back i.e. two jars, lids on, one yellower than the other.

I remember spices technique of titrating to ph6/dry acetone etc. could I perform this route then?

I was going to set up to form hcl gas via psychokitties post using sulphuric acid and 33% hydrochloric.

igt

T-cowboy

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Re: Jon's route
« Reply #57 on: July 30, 2012, 11:18:49 PM »
Yes evap that off! until you can not smell anymore alcohol.. then add equal amount of water (of whats left in the flask, and that should be yellow/brownish coloured mixed stuff)..

Then basify to ph 12, and then extract with some solvent.. ( if you want ) separate that solvent/freebase, then evaporate solvent away (again, yes)

You should be left with an oil.. imagination from here on..

I also need to know, how much methylamine gas you bubbled into your COLD IPA?

And how much iodosafrole you ended up with?


here follow this : http://127.0.0.1/talk/index.php?action=dlattach;topic=1697.0;attach=3276
« Last Edit: July 30, 2012, 11:26:17 PM by T-cowboy »

igotthere

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Re: Jon's route
« Reply #58 on: July 31, 2012, 04:53:37 PM »
ok thx, although having talked to spice I'm now very much favoring his route rather than gassing.

I had approx 10g of idosaf, I was aiming for 16g methylamine in my ipa but I think I ended up with lots more as I was using dry ice. I can't give an end weight as I was getting in a fluster towards the end of the gassing and forgot to measure final weight...

Am hoping to work it up tonight

igt

T-cowboy

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Re: Jon's route
« Reply #59 on: July 31, 2012, 06:57:20 PM »
YEs gassing can be a bitch.. how is your method for getting the hydrochloride if i might ask?

Looking forward for your results, as i have been trying to get this reaction to work for 1 year actually..
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