Jon, did you ever use Nal instead of Ki? are there any pros/cons to Nal?

Am about to give this another go

IGT

NaI is much more soluble in acetone (28g NaI per 100g of acetone compared to 1.66g KI per 100g of acetone) so it will react a lot faster with less stirring needed.

Yeah you should still use a molar excess. The numbers I posted are the amounts of NaI and KI that will dissolve in 100g of acetone at room temperature so you could see why NaI is better to use as more will be available in the solution for bromosafrole to react with. NaI is a lot more expensive than KI and both give the same yields in my experience. With NaI the reaction just occurs faster with less stirring needed for completion. The reaction is also much more apparent when using NaI as you just need to look for NaBr precipitation rather than a change in the look of the crystals present in in the solution.

thanks guys, have had my Nal for a while now, just haven't had any time.
 
My bromo went really well, almost 20g bromo from 20g saf. nice and dark in colour.

covered up in a sealed jar at 0degc.

hope to progress to ido early this week.
igt

a little update - haven't had the time to do my finkelstien yet but I did do a quick test using freezer cold h2so4 and a drop of my bromosaf.

The second it hit the acid it spread out really quickly and went a predominently dark browny rusty colour with slight blood red tones, but no visible purple shade.
The colour range was from a very dark brown to a rusty/deep blood redish colour. it didnt sink either.
I swirled it after 30 seconds and saw a sort of oxidised darker section forming, plus some wisps of vapour/gas? 

jon - would the purple colour be quite noticable? does the colour range I'm seeing sound right?

hoping to go to ido next week now

igt

Do the same test with safrole and see! Its quite apparent yes. Sounds like you got the greenlight for actuon bro

I ran my finkelstien reaction and I'm cautiously optimistic!

I had 20g bromosaf.

I added 16g (1.3x molar amount) of Nal to a 100ml rb flask then added acetone (not fucking IPA like last time... ) until it all disolved.

I then added the bromosaf and spun for 30mins.

Added around equal volume of water, spun briefly then added around 30ml DCM.

Spun for 30 secs then dumped it into a sep funnel.

Removed the DCM/oil and extracted the water layer with another 30ml DCM.

Combined the two DCM's, washed with water then evapped off the DCM in a small pan to recover 16ml of very dark oil.

Now for the colour - I have it in a measuring cylinder and at a glance its very very dark almost black, but as you tilt the cylinder and shine a super bright LED pen light through it from underneath you initially see a yellowy green colour at its thinnest outer edge, that slowly becomes a definate purple colour before the light dissapears completley.

Idosafrole?

igt





 

The color sounds right. Does it smell more chemical like?
I noticed the Bromo smells very sweet and the Iodo smells more like vick's vapo-rub.

Looking forward to your results..

Snap!

Good to have someone running along side me!

igt

igothtere.

you have iodosafrole dark purple chemical odor nothing like bromosafrole.
you can heat it with ammonia with methylamine heat will just E-2 wliminate HX and it will turn to tar so room temp works fine when you add it it 8 moles of methylamine in ipa at 12-15% concentration it will almost instantly convert to mda or mdma it's a sharp transition when you get it right nice work there man you'll be turning it out real soon.
it turns piss yellow evap all down the drain with an aspirator then acid base workup and you got the goods my yeilds are so high i just extracted and washed it with water evaped solvent then add equimolar acetic acid and then one volume ethanol and 2-3 volumes of acetone = translucent crystals.