Hi all,

As I just mentioned in the 'yeehaa' thread I have some free private time coming up soon. I'm very much a believer in Jon's route, so I want to have another good go, but I'm looking for as much help as other bees will be prepared to give in order to remove as much potential for error.
 
Hopefully this request for help won't be seen as a newbie trying to run before he can walk. I certainly wouldn't call myself a 'chemist' but, in the few years since I've known about chemistry and its wonderful dirty underbelly, I've managed to successfully acquire everything needed to run benzo wack - al/hg's to completion with fairly good yields, so I think I've earned my first gold star. But Jon's route is just sooo alluring... to get this working would be fantastic.
 
Some of you may have seen my efforts over at pn in Spices 'Revisiting Halosafroles' thread. I didn't get anywhere regarding end product, but I do have EVERYTHING needed to effectively run this route, including methylamine hcl and, in a weeks time, dry ice.
Previously I've successfully managed go through the physical process of brominating safrole, but I'm unsure as to if I ever got to actual brominated safrole. I did successfully manage to dissolve methylamine gas into (ice chilled) IPA using a home brewed 'ghetto gas generator' ala Jon's tech (complete with disposable enema..). I saw a change in weight of the IPA from start to finish, so I'm taking that as a successful run.

What I am definitely sketchy about is my math. So my first request would be for someone who, hand on heart, can actually do the math!
I have genuinely given it my best shot and will post my figures here, but this is obviously an area where some big errors can be made.
So to have correct stoichiometry from the outset would remove any potential for error here.
Also with the stoichiometry sorted out the only other room for error will be all down to me! So I'll happily take the blame for the anything else..

igt

Good Luck, you're kind fractal.

thanks, fractal you have a PM!

carl, yes I have that somewhere, is in the 'yeehaa' thread I belive

igt

Bee careful when washing your DCM extracts of the bromosafrole with sodium bicarbonate. It creates an emulsion and the problem was left unaddresssed without closure in te yeeeahhh thread

Edit: it may not be necessary! I'm not an expert on the matter, but every writeup ive read includes the bicarbonate wash.

Goodluck!!

Let us all know if you get honey! And post pics!

thx ImaMAN.
Am assuming that the bicarb is to neutralize the GAA? Jon talks of adding bicarb until the fizzing stops.

That's the idea! But apparently it can cause nasty emulsions.

I think jon recommends TCE break cleaner since DCM has this problem...

I used ether, no emulsion formed.

thx, I'll look into TCE but are there any other options to neutralize the gaa?

You can still use sodium bicarbonate to neutralize the GAA as long as you are not using DCM. Ether, Hexane and TCM should work in DCM's place.

(much thanks to fractal for the information)

I think jon recommends TCE break cleaner since DCM has this problem...

I may not be 100% correct by saying this (I recently PMed another member to ask!) but TCM's boiling point is 80C above what DCM's is and may be less suitable than ether or hexane as a replacement 

out of my mind, tcm boils below 60°C and dcm below 40°C
ok, could be 80°degress in fahrenheit, im not sure, every chemist should ban this fahrenheit crap immediately out of his brain!
tcm is anyway because of its other name chloroform and its widespread knowledge about the most hard to get out of the list hexane/dcm/tcm/diethylether/mtbe

out of my mind, tcm boils below 60°C and dcm below 40°C
ok, could be 80°degress in fahrenheit, im not sure, every chemist should ban this fahrenheit crap immediately out of his brain!
tcm is anyway because of its other name chloroform and its widespread knowledge about the most hard to get out of the list hexane/dcm/tcm/diethylether/mtbe

Hardest to get where? In the US you can get it otc in hardware stores...