really in hardware stores?  in europe never, and any other chlorinated solvent is hard to come by too OTC, because we have working environment protection laws...
ever heard of organic layers in rivers underneath the water layer?
i mean because of industrial waste getting dumped in or even worse with a direct flow straight from a factory, its more common in the states, as it is in china too
nowadays more of a past problem luckily but it has happened...
its really horrible to imagine a river who owns his own dcm/tcm/freon layer isnt it?

ever heard of organic layers in rivers underneath the water layer?

thats really fu**in scary! never thought about that possibility... ^^

bromo is plenty stable unless you heat it

What percent concentration of HBr did you create in the GAA? Someone suggests 50 but isnt this a bit high?

fractals comment on percentage of hbr:

'I try to keep the acid strength to the min needed as HBr can cleave ethers.'

I wish I knew what that meant Fractal!

Anyway I ran my bromination on Saturday at 9am. I chilled my GAA to just around freezing point, added my NaBr and saw a slight change in the colour of the GAA. It turned a sort of grapefruit juice colour- kind of a very pale pinky yellow.
I Chilled again then added my h2so4 at a steady fine pour, not dropwise. There was some slight heat evolution that could be felt through the glass of my pesto jar and I instantly got the trademark deep orange colour with some slight traces of hbr fumes.
(acquisition tip: sigma aldridge sell a wide range of pesto jars, as do most supermarkets...Its wise to remove pesto first)

I added all of my h2so4, swirled gently to mix, popped the lid on, wrapped in foil and popped it in the fridge while I sorted out my chilled safrole.
I then added my safrole and had another instant colour change, this time to a deep purple with hints of brown, sitting as a layer on top of the orange GAA/Hbr  and gently sending little wisps of purple down into the orange.
I didn't choose to swirl at this point so I wrapped in foil and placed the jar in the freezer.

Fast forward and I have now removed the jar from the freezer. The mixture wasn't frozen solid like it has been in the past, although I'm sure that was due to my poor maths. This time it was a nice uniform deep purple colour, no orange at all.
I thought I could see some separation going on.
I decanted the fluid from the salts. There was some slight hbr fuming, hardly noticeable really other than smell.
Jar is now in the fridge.

Thats where I am right now.

Thx carl.

Regarding the use of DCM and its tendency to form emulsions, and at the risk of sounding like a complete dick, could I not just suffer some losses by not extracting the first water layer and going directly to washing the bromosafrole/GAA mixture? so I would do points 1-4 below, then jump to point 8 but without any solvent to worry about forming emulsion?
I know this is wasteful but I don't have any TCM or ethyl yet and I'm keen to see if I can make this work, less worried about perfecting yields at the mo.


1. throw the shit in a sep funnel
2. add 1-2 volumes water
3. let the bromosafrole crash
4. sep it out
5. extract the water layer a few times (gauge by color)
6. combine the solvent with the bromosafrole
7. discard the acid/water
8. wash the solvent/bromosafrole with water adding bicarb and swirling until fizzing stops
9. dump this wash
10. wash with water then brine and instead of losing product to volitization in the dessicator
      try drying the solvent/ bromosafrole and filtering using a drying agent like mgso4

jon now is one of those times a little input would probs help.. let me tell you if you have bromo safrol, word is it will evaporate fast.. jons word is if you take your eye off it for a while comeback there is half the amount left..  you wanna  make sure everything is well calculated before you proceed

just a point to note on colour, the oil looks nice and dark brown so if thats anything to go by I'm hoping this signifies bromosaf

nice one jon, have just done that. I included a brine wash. I have some nice dark browny coloured stuff that looks suspiciously like bromosafrole.

So now to idosafrole:

Please anyone chime in but I'm planning on doing the following to get to my idosafrole:

After calculating how many moles of bromsaf I have I plan on drying my bromo with mgso4 by simply adding to my jar. I will then add to some finely ground Ki and add dry IPA until its stirable, then spin the shit out of it for 40mins.

workup of ido would be add water until salts dissolve and oil drops out, then extract with DCM, wash and evap dcm to get my idosaf.

Any advice be before I get going?

igt

you have 13g Bromosaf which are 0,053 mole ( 13g/243g/mol). So you need (166g/mol*1.1 mol * 0,053 mol) 9,76g KI. So your calculation is right. 

right so I flooded with water until the salts dissolved, then extracted twice with DCM.

I then evap'd the DCM ghetto style with hairdryer setup.

I have a dark brown oil with a slight purple edge.. I wouldn't say its predominantly purple by any means, but theres a purple hue.

Interestingly when I cleaned out the jar that I'd used in the extraction process I used a piece of white kitchen roll. I wiped it round the inside of the jar and there was clearly a dark purple colour on the tissue.

Is now in a small jar in the fridge.

Dry ice comes this week so hopefully I should be able to move forward to enriching some dry IPA v soon.