Well, I think a 10x (1 mol) ala Chromic in the five gallon bucket is looking pretty favorable, as long as the stirrer can move 10L solution...
How bad are the smells with this? I would think the "Pool Shock" would overpower most/all odors, at that temp (< 40C)...
PB
1) Add 162g stuffrone into 14L bucket, and dissolve/wash flask/add 2L MeOH.
2) To this, while stirring heavily, add 5L dH2O and 727g oxone (sediment filtered/cleared prior).
3) Slowly, add 244g NaHCO3, and let contents stir for five hours, with no external heat (kept 40C).
4) Turn off stirrer, let mixture settle; pour contents into beaker w/o any solids; vacuum filter crystals out; wash with MeOH until bright white.
5) Load into sep. funnel and extract 3x 1L DCM(recover DCM with water bath) .
6) Then add syrup to 3L flask with 250ml MeOH, and gently heat to ~ 80C.
7) Bring 1.2L H2SO4 (15%) to 80C, then quickly dump in the flask, with hard stirring already initiated.
Lightly reflux for 3hr at 80C(temp change from 72-85C; steaming, but not boiling), then allow flask to cool, and the mixture will go from light yellow to darker brown.
9) After at room temp, add to sep funnel and seperate off crude stuffrone (on bottom; D=1.2), and extract acid in funnel with 3x200ml DCM, and combined with other seperation.
10) Wash 3x 800ml NaOH (5%) , first time gentle rock, next two shaken (black light to determine layers; stuffrone green, on bottom; should take reddish brown color out).
11) Distill off DCM in oil bath, and distill over stuffrone at 20C more than stuff (i.e. 120C would become 140C, under reduced pressure).
