Well, i answered my own question: HBr does not dissolve teflon tape. After a nasty 2 hour session SWIM has a bunch of 48% HBr from some pool sanitizer(NaBr) and some drain cleaner.
Here's some stuff from the old board that might be useful to someone:
Safrole-azide:
"In a one-neck flat-bottom flask on a stirplate[turned on] are combined 100g bromosafrole , 30ml dH2O and 50g NaN3. 5g butylamine are dripped in. Then a condenser is attached, the soln brought to reflux and kept there for 6h. After cooling, extraxt with Et2O, dry thru Na2SO4 and distill off the ether to get the Safrole-azide. Yield is 75%. You can get near 100% if you take 'aliquat 336' as PTC. without a PTC yield is only 50%.
Reduction:
200g safrole-azide is dissolved in 1000ml MeOH and 100g SnCl2 [or the dihydrate] are scraped in in small increments.Almost imediately heavy bubbling and heat will evolve. This is released N2, tells you that everything works. Then let stir for another 60mins. Remove the MeOH by vacuum distillation. To the remaining oil add 500ml ice cold dH2O. Bring the pH to 9-10 by addition of dilute NaOH soln. Saturate with NaCl. Extract with ether, wash ether extract with NaCl soln and dry thru Na2SO4. Remove solvent by distillation. Yield is 98%."
I like that SnCl2 reduction method, looks real simple if you have some SnCl2.
WizardX: your recipe uses EtOH as the solvent for making the safrole azide at 50C. Could this rxn be done at 65C in refluxing MeOH? Should not make a difference if it is MeOH or EtOH, or even IPA right?
Any specific reason for using the ethanol?
Would the bromosafrole still dissolve if 50% EtOH was used or would it be a 2-phase thing?
Shit it's getting kinda late and I need a coffee.
Any tips on the solvent issue appriciated;
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--improv
It's all just a dream, I hope i don't wake up because of that incessent buzzing sound...