Here's what SWIP is dreaming of dreaming in a few weeks:
A) Distill
· Add .5g Hg to each (
tincture bottles for 3days min.
1) Use grease on joints, insulate up to column with foil, room temp water through column, give air-leak when heating without vacuum.
2) Add 250ml stuff with to 500ml RBF, 250ml RBF receiving.
3) Slowly bring stuff to 130C to boil off water, with stirring, till no steam is left, then bring up to 234C (BP of stuffrole), and let cool to room temp.
4) Begin vacuum slowly, with heavy/fast magnetic stirring, then slowly bring to ~121C (depends on vacuum; see bottom).
5) Try to get 5-10 drops a minute, and do not go above 160C (try to keep 5 degree range for distillate), do not distill dry.
6) Use safflower oil bath, in aluminium or copper bowl with stir bar in oil bath, along with one in flask, flask not touching bowl.
*About the first 7-10% of the distillate is crap, the next ~85% is stuffrole, and the deep red shit in the boiling flask is more crap.
B) Isomerize
*Start peracid sometime 12hr prior to being done.
1) Fit flask with reflux condenser with vacuum attached as per distillation.
2) Add 3g KOH in small portions to 200g stuffrole, then bring to reflux under vacuum (130C) with damp-rid in condensor and receiving flask.
3) Reflux for 10-12hr (boiling will be smoother when finished), and then turn off heat, let cool 2hr.
4) Heat stuffrole to BP, then allow flask to cool, and change receiving flask and wash with acetone.
5) Begin vacuum slowly, and distill isostuffrole at ~ 136C (15C over stuffrole; ~ 240C bath temp).
C) Oxidation
1) Add 650ml AA(90%), 140ml H202 (25%), and 8ml H2SO4(32%), to 3L RBF, stopper flask, and shake thoroughly.
2) Once well mixed, let sit 11hr, then chill 1hr in fridge to 20C min.
3) Add 140g isostuffrole with 220ml acetone, then chill in freezer (~5C).
4) An ice/salt/water bath used to keep flask cool, ~ 5C.
5) Slowly add isostuffrole/acetone solution to flask (~35min), with good stirring, keeping temp below 20C (temp stabilizes after ~1hr).
6) Remove ice bath, let stir for 16hr (keep flask temp 20-30C).
7) Add flask contents to 3.6L water, then separate glycol/epoxide, and extract this with 3x with 210ml DCM (may break down into three portions; if emulsion forms with DCM, use a little salt to break up).
Wash with dH2O, strip off DCM and save for step 11, then add syrup to 2L flask with 200ml MeOH, and gently heat to ~ 80C.
9) Bring 1.1L H2SO4 (15%) to 80C, then quickly dump in this syrup, with hard stirring.
10) Lightly reflux only for 2hr (75C-80C; steaming, but not boiling), then allow flask to cool, then flood with 500ml dH2O, and set in cold water bath for 20min.
11) After at room temp, add to sep funnel and seperate off crude stuffrone (on bottom; D=1.2), and extract acid in funnel with 3x180ml DCM, and combined with other seperation.
12) Wash once with 500ml dH2O, then once very, very easily shaken with 500ml NaOH (5%) (use black light to determine layers; stuffrone green, on bottom).
13) Strip off DCM, then distill stuffrone at 25C more than isostuffrole temp (135C-150Cmax).
D) Animation
1) Carefully add 60g aluminium and 1.5L MeOH to 3L RBF, and heat to ~ 55C (made before hand by adding 2x tincture bottles to 500ml dH2O + 500ml MeOH with 60g Al, allow 17-30min to react, until grey precipitate forms, likely to be 30 mins, decant liquids, wash foil with dH2O, then with MeOH; do not expose to air after, store in 1.5L MeOH).
2) Carefully pour 40ml MeNO2, then 80ml MeOH, then 50g stuffrone to addition funnel, and set into position.
3) Place 500ml condenser with, optional steel wool, into position; run off heat; start drip rate at 3dp/sec carefully, letting stirrer stay on constantly, 2dp/sec set after.
4) Try to come to the peak, back off a sec, and then finish addition before amalgamation is done (~ 30min)(try not to let rxn run-away; there is little un-dissolved Al when done).
5) After 2hr from initial addition, may need to add more MeOH, then let contents reflux for 3hr, then cool for 30min.
6) Make NaOH (35%) (mix 530g NaOH per 1500ml water or ice), make sure cool, and slowly add to flask with use of addition funnel.
7) Let stir for 1hr, then add 900ml xylene to 4L flask, or split into two batches, then decant xylene, and wash contents of flask once more with 200ml more xylene.
Chill xylene in freezer for 30 min, then decant, leaving garbage in flask.
9) Wash out sep funnel, then add xylene solution, then wash 3x dH2O (1L) or until clear, then 2x with brine (1L), then once more with dH2O.
10) Add 60g MgSO4 to xylene in container and shake, then let sit 30 mins.
11) Filter out MgSO4, wash filter cake with fresh xylene
Crystallization
1) A/B extract (50ml dH2O + 5-6drops muratic (pH 6), dry until syrup, crash out with ice cold acetone, followed by 2x ice cold acetone washes.
2) (*Optional): Dissolve in minimal amount of hot, anhydrous IPA, let cool to room temp.
3) Add 2x acetone, then seal and place in freezer for 12hr.
4) Filter out crystals.
Any last words of advise? Should he buffer peracid with sodium bicarbonate, or could this induce any side-rxns?
PB