Oxone yeilds

[goiterjoe]

Are you not distilling your ketone?  if not, how can you possibly be bitching about yeilds!?

[lablozer]

vap'd off = distilled

Sorry SWIMMER should be more specific when drunk.

[Vibrating_Lights]

The buckets make great rxn vessels don't they.  Just remember it is possible to get a 8-10gallon bucket similar to a paint bucket.
VL_

[SuperStar]

Hey VL or someone,

When doing the oxone in the bucket. 

Are there any good tricks or tips for getting the epoxide out of the bucket with minimum DCM?

What about filtering the oxone solution before hand?

Guessing to get 2 or 3 buckets and try to filter back and forth between the two until the solution is clean. Then starting DCM, dunno, need some ideas?

You guys using a 5gal or a mop bucket (3 gal) for the 10x oxone.
Pardon my friend officer, He's a little slow.

[goiterjoe]

Has anyone tried flooding the post reaction mix with, say, 4x the amount of water to get the mix to separate better?  I've wondered if the salts that fall out of solution will go back in if the methanol concentration is lowered substantially.  Anyone willing to try?

[Vibrating_Lights]

When the rxn is flooded with water it does help to get the epoxide out to the bottom.  On a large scale  let the oxone solution settle. put 50% of your DCM in another bucket.  Then Pour the oxone liquid into the second bucket and either stirr or pour back in forth in another bucket.  Then do like chromic says and wash the crystals with some MeOH and add it to the dcm/toplayer.
VL_

[SuperStar]

Hey VL,

When you say put 50% of your DCM in another bucket, what are you doing with the other 50%?  SWIM knows this is stupid question but got confused.
Pardon my friend officer, He's a little slow.

[GOD]

seeing how VL has supposivly ducked out, can anyone give a theoretical awnser to the last question?  Swiy is fixun ta give the oxone a whirl and is 'studying up' for pointers etc...would the other 50% get used to washout the other bucket after its been emptied?
when someone asks what the sound of one hand clapping sounds like, you should smack them in the ear.

[SuperStar]

VL, must be doing the 50% in a bucket twice. Sort of like extracting 2x50% DCM

Just a guess.
Pardon my friend officer, He's a little slow.

[SiLiCoN7]

Don't worry about the other 50%, Extracting the oxone is easy. Just filter then extract the whole lot together at least 3 times with DCM. Two big 5L DH2O bottles are good, just shake, settle for at least 5 min, decant the majority into the other bottle then transfer to the sep funnel for seperation. The DCM is almost clear on the 4th extract.

Combine extracts and wash once with about half the volume of DH2O to wash away any oxone remnants then evap the DCM.

If you don't filter the oxone before the reaction, the white powder will continue to percipitate with each extraction, even after post reaction filtration. SWIS7 believes that this is a result of the pH changing as the epoxide is removed. Is this correct? Anyway, don't worry about the percipitate, it will dissolve with just one wash at the end.

the 21st of the 12th 2012......