I haven't finished making methyamine myself yet.  I have worked up some xBee said didn't react completely before deciding to try for myself.  It is confusing I know.  The first batch he did, dodn't get enough methylamine in.  2nd batch I don't think water may have been the problem.  IT takes us forever to do things.

Salat

always tare the weight of the alcohol and the vessel you gas into and make sure you combine whatever is in the suckback trap with the gassed solution weigh this to determine the number of moles of methylamine, or ammonia and, the solution concentration then, use the 8-10/1 ratio methylamine to halosafrole.
the concentration can be as low as 10% and it will still work. (w/w concentration of methylamine dissolved in alcohol)
make sure your calculations are straight before procedding.
15/1 is the ratio for ammonia.
in gram moles.

Can't comment on the reaction since I'm not familiar with it, but nice work and pictures !

I will still add with pretty much confidence that you won't end up with nothing even if you fucked up on the safrole ratio as it's not the limiting reagent for sure  . Depending of the reaction's mechanism,it can changes something or NOT, I can't tell for sure. 

Yeah,it's great method,we thought the same thing about write-up!
More people do it,the better!
Only thing that stoped me from doing that reaction before was lack of sassy and time.

You can't overbrominate unless you expose too much to UV,head and some catalysts and what not...
Jon also mentioned multiple times to add all safrole at once and don't stir.

After how long your safrole changed color!?

Keep us updated!
Good luck!

After 22 hours the reaction had turned a very dark red colour, almost black. On removing the flask from the freezer I carefully decanted off the majority of the solution into a beaker. I then added approx. 300ml of water to the flask to dissolve all the residue and salts still in the flask. This was then added to my 1 litre separator funnel and the organics were extracted with 3x75ml portions of DCM until the water layer was cloudy but colourless.

The DCM extracts of the residue were combined in a beaker. The water layer was then discarded.
Next approx. 500ml of ice cold water was added to the decanted Bromosafrole which was placed in the separatory funnel. The Bromosafrole was then extracted with 150ml, 50ml and 25ml portions of DCM till the water layer was again colorless.

Both of the DCM extracts were then combined in the separatory funnel and washed with 300ml of water.
Following this I proceed to wash the DCM extracts with a sodium bicarbonate solution to neutralise the GAA. Then something terrible happened! I got an emulsion! I tried breaking it up with brine, by adding more water and more DCM without much luck. I'm stuck with a lot of pale yellow emulsion which is refusing to separate back into the nice brown bromosafrole layer. Anybody have any ideas how I can fix this? I have the mixture left overnight to see if it separates. I have a feeling it might have something to do with temperature as my lab is unheated and the temperature drops too about 6-10c. Could that make a difference?

Also would it be possible to use CaCl2 to dry the product as I don't have any MgSO4 on hand, although I should be able to get it if needed.

Thanks in advance for any help!

I don't understand this part:

Next approx. 500ml of ice cold water was added to the decanted Bromosafrole which was placed in the separatory funnel. The Bromosafrole was then extracted with 150ml, 50ml and 25ml portions of DCM till the water layer was again colorless.

I suppose you're washing the decanted bromosafrole with that water, but I don't get why you extract it with DCM when you could just proceed to the next step directly.

Don't bother with that next time 

Great work and pictures again by the way. Looking forward for more By the way, how is it going with the methylamine synthesis?

I'll let it sit for 24 hours, if there is no progress, I'll try heat the mixture and hopefully that would do the job!
I haven't started the methylamine synthesis yet, I might have a go tomorrow while I wait for the emulsion to separate. I'm planning on using the hexamine/hcl method to generate the methylamine though I'm still a bit unclear about the method. Anyone have any tips I should know?

Finally I don't have any molecular sieves atm, would I be able to get away without drying the methylamine/IPA suction if I start with reagent grade IPA and I am carefully with the gassing?

Finally I don't have any molecular sieves atm, would I be able to get away without drying the methylamine/IPA suction if I start with reagent grade IPA and I am carefully with the gassing?

There is no careful with gassing, it produces water and heat which lead to water vapor. If your not gonna dry it all the way it's pointless from what others have said. Sieves cost $12 for 100g, well over worth what swiy'll lose. You can get anhydrous electronics grade IPA (99.953%) for $26/gallon.

dude !
first learn stoichiometry
80.1 g h2so4= .952 g moles h2so4
and
80 or so grams of nabr is like .77 g moles of nabr
you have a shit load of sulfuric acid floating around that can wreck your safrole.
but a testament to this method is that you made that boneheaded mistake and still got product.
potasium carbonate is typically used but it does'nt matter just wash the acids by adiing equal water and dropping bicarb and swilrling until the fizzing stops
wash with water then brine
that's it.
it will be dry enough.
next time run it by me.