pH checking of Oxone

[noj]

Swim has been trying to monitor the pH of the oxone while adding the bicarbonate. I have this feeling that the evolution of bubbles is giving a false pH reading (using strips). Regardless of the amount of bicarbonate added he always gets a reading of pH 8. After the 5 hours a final reading gives an acidic 5-6 unless the total amount as Chromic suggests is added.

The solution at the end is supposed to be a yellow tint, but lately it is orange. The orange also fails during the amalgamation. Since it worked before I started fucking with the pH it is apparent that the oxone swim uses is 100% and that Chromic's writeup is the one to follow.

So, how could one get an accurate reading of pH?
Real men cook naked.

[Vibrating_Lights]

The Ph of a saturate dsolutio of Oxone is 2.3-3.  if your oxone is pure then definatly use chromics ratios.  the reason Swim mentioned the checking of the Ph Is becausesome people are not working with pure oxone.
VL_

[noj]

Would being acidic cause the orange appearance?
Real men cook naked.

[Chromic]

My oxone trials on isosafrole gave a yellowish-orange epoxide. Follow the writeup as written, change only one variable at a time if you wish to change anything at all in it (so you can see what to change if something does go wrong). Use the bicarbonate buffer when using oxone, it makes it a stronger epoxidizer. Don't play with pH.

[Vibrating_Lights]

Swims oxone works well straight out the bag because of sodium carbonate added by the manufacturer to give a ph of about 6.7-6.9.
VL_

[PoohBear4Ever]

What's the maximum weight of iso one can react per liter of flask for this method(...16.2?))?

PB
concoct: 1) to prepare by combining raw materials; 2) to devise or fabricate

[Chromic]

About 20-25g iso/L.

[PoohBear4Ever]

Heh, so if we could modify baalchemist's 55 gallon Al/Hg method to work with oxone...

Seriously, though, that's not too bad, considering the benefits of OTCness of it...

PB

[Chromic]

If you want to be OTC and make a lot of ketone, use GAA/H2O2/DCM or formic acid/H2O2/DCM. If you want a small bit of easily made ketone, go with Oxone. I don't see the reasons why people would want to scale up a synthesis which isn't volumetrically efficient.

[Vibrating_Lights]

1620 Gms isosafrole & 20L MeOH is loaded into a 55 gallon barrel with a teflon coated boat propellar mounted on a coated steel shaft.  Heavy stirring is commenced  Then 50 liters of dH20 and 14.2Lbs of oxone.  4.76 lbs of sodium bicarb is added slowly over the period of 10 minutes.  If pool grade 85% oxone is all that is available then it is nescesary to omit the sodium bicarb as it would bring the Ph to high. and 16.7 lbs straight out of Then bag will be nescesary with no base. Stirring is run for 5hrs,  unless you can some way seal the barrel with a teflon bearing on the propellar shaft and add a 2atm pressure release valve,  in which case a rxn time of 3.5hrs will give similar yeilds as a standard atm oxidation. There will be a valve at the bottom of the barrel to drain the solution through a few celite pads to catch any percipitate. before opening the drain lean the barrel away from the drain so no percipitate will get through till almost the end. Celite pads are the shit.also useful in completely filtering an Al/Hg in as much time as it takes you to safely pour it through the filter. When all of the liquid is gone the valve is closed and an additional 2 gallons of MeOH is poured in the barrel and drained through the filter.  under the filter will be a another 50 gallon barrel with 10 L of dcm in it.  after it is fullstir for a few minutes then drain off the bottom layer into 20 galon barrel.  extract 2x more with 10L dcm draining the bottom layers into 20 gallon barrel rig your barrel up on two of the big hotplates from wally world in a water bath and distill off the dcm keeping it for the next extraction.  then add 2.5 liters of MeOH and 9L of 15% H2SO4.  Reflux for two hrs  when the solution has cooled roll the barrel towards the drain and drain off the crude ketone into a 20 gallon barrel. close the valve and add 10L DCM stirr and drain.  then 12L DCM stirr and drain.  WASH DCM extracts with 800 ml 5% NaOH 3x or until dcm is clear.  If you plan carefully you can install a second valve on the barrel a litle above where you expect the seperation line to be so you can just drain off the top layer.  when draining off the final wash more dcm can be added untildcm is coming out the valve. Distill off the DCM in the 20 gallon  and drain the ketone into a n insulated 4l rbf and distill under vacume.  What to do with all that ketone? stockpile it and aminate it all at one time in the community pool with the Al pool furnitureGod Oxone is great. sOO CHEAP. cELITE cELITE cELITE.  IT IS EVEN EASIER THAN THE MDP2POL THING WOULD HAVE BEEN.
P.S. If you elevate your barrels to the proper positions prior to use the proscess is as simple as flipping switches and opening valves  mount stock solvent tanks high so you can have hoses to dispense instead of pouring.  full computerized automation is as easy as a computer programs and electronicaly controled valves.  thermal reearangement at this scale has not been attempted.
hAVEFUN bEE SAFE
VL_ 

[noj]

PB, using a paint style 5gal bucket, one could epoxidize 450g isosafrole. Little heat gets produced so the bucket works great. After that, everything get's scaled down to the 1-2L flasks.


Real men cook naked.

[Vibrating_Lights]

swim does not believe it could be done in a f gallon bucket  there is more water needed to dissolve the oxone.
VL_
P.s a two liter shows no signs of deterioration for a batch on the fly KRVStyle

[noj]

Well I guess swim should wake up because he is looking at 350g of a nice yellow fluid sitting in a freezer, and that can't be.
Real men cook naked.

[LaBTop]

  LT/ L.O.V.E.S chemical ingenuity, eh, engineering!      
WISDOMwillWIN

[PoohBear4Ever]

Ahem, I take it if it's still a fluid in the freezer, this is the ketone one seeks?

Very interesting suggestion, indeed,

PB

edit: "The color will change from a swirling mix of white solids in a colorless and clear liquid to white solids in a light yellow liquid." <-- I guess so...  

[PoohBear4Ever]

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).

[noj]

An old 7x7 Corning had no trouble making a vortex 2" wide with a 3" stirbar. Make certain it is centered well and spinning full blast before adding the dry goods.
Real men cook naked.

[Vibrating_Lights]

Smell of reaction in general is negligable.  pour the post rxn mix through a couple of pads of celite in a funnel then only an minimal ammount of methanol mustpoured through filtercake.  celite is the shit for filterring al/hg post rxns .allows for quick clean workup and there will be no sludge in the dcm.  SWim says go for the full 10moles alkene and go it in the barrel.  With the cost of the regents. 25lb buckets of oxone for $50 properly rigged barrels for under $20.  The future is here. 
VL_
Super condensor core in a barrel
_____________________________________-
 a refrigeration system is removed from an old refrigerator in tact and the coils are thinly coated to resist solvents.  the cooling coil is mounted in the top of the barrel and thermostat set properly.

[PoohBear4Ever]

...a couple of pads of celite...

Do you mean multiple layers of celite/filters, or multiple seperate filter cakes?  Thanks for the tips...

PB

[Rhodium]

Where do you buy your celite? It is hideously expensive from Aldrich...