Author Topic: Oxone or Performic/Peracetic  (Read 26460 times)

0 Members and 1 Guest are viewing this topic.

aznxprophetxtasy

  • Guest
Oxone or Performic/Peracetic
« on: June 10, 2002, 12:51:00 AM »
Hello,

Since I am a New"bee" and this is the Newbee forum i am going to ask a newbee question.

In terms of yield which is better Oxone or Performic/Peracetic. In terms of easiness which is better??



greeter

  • Guest
Performic
« Reply #1 on: June 10, 2002, 01:00:00 AM »
UTFSE.  The performic yields ~85%, the peracetic according to Chromic can yield ~70%, the oxone route maybe 50%?  Seems to me most people have been having problems with the oxone route.

A watched pot will indeed boil.

Chromic

  • Guest
Not quite
« Reply #2 on: June 10, 2002, 01:42:00 AM »
The buffered performic yields 65-75% of theory.
The buffered peracetic yields >60% of theory (likely 65-70%).
The oxone method yields 50-65% of theory (perhaps higher).

The main yield limiting step is the sulfuric acid hydrolysis, tosic acid may give higher yields. As of yet, no one has posted any information on the topic.

aznxprophetxtasy

  • Guest
So im guessing here since Oxone uses loads of H2O ...
« Reply #3 on: June 10, 2002, 02:04:00 AM »
So im guessing here since Oxone uses loads of H2O that performic is the best option. Also i looked under the search engine and found the yields to vary. i just wanted some other bees opinions. Thankx!!

greeter

  • Guest
performic yields
« Reply #4 on: June 10, 2002, 03:18:00 AM »
Swim's last three performics ran with 82%, 87% and 87% yield respectively (w ketone / w isosafrole).  Swim was *very* careful with everying including a fractional distillation at the end, making sure to get out all water, dcm, etc., and toss the forerun which came over right under the ketone (which was about 30 drops of something very ultra-neon-green, coulda been ketone but...).  The rest was bright yellow.  85% avg.


A watched pot will indeed boil.

hypo

  • Guest
yield is allways molar!
« Reply #5 on: June 10, 2002, 03:31:00 AM »
> Swim's last three performics ran with 82%, 87% and 87%
> yield respectively (w ketone / w isosafrole).

come on! you know that yields are (actual / theoretical).
so your 85% is really only 77%. probably not ultra pure
and you get the values of chromic...

Rhodium

  • Guest
Hypo: Are you suggesting that greeter calculated ...
« Reply #6 on: June 10, 2002, 04:21:00 AM »
Hypo: Are you suggesting that greeter calculated a weight/weight yield instead of a mole/mole yield, or am I completely off?

hypo

  • Guest
yes, i think so.
« Reply #7 on: June 10, 2002, 04:25:00 AM »
yes, i think so.
at least that's how i interpreted  "(w ketone / w isosafrole)"...

Rhodium

  • Guest
molar yield!
« Reply #8 on: June 10, 2002, 04:32:00 AM »
Oh, sorry - I didn't see those w's.

Why is it so hard to calculate the molar yield, everybody? The molecular weights of all the compounds we are using here are plastered all over the web, and is automatically calculated by programs such as ISIS-Draw... And all this just if you don't want to learn H=1, C=12, N=14 and O=16, and perform simple addition and division.

SiLiCoN7

  • Guest
Which is better?
« Reply #9 on: June 10, 2002, 11:10:00 AM »
SWIM runs oxone at about 55% crude weight. Oxone is whaaay! easier IMO and gets cleaner products if you don't own a ketone distillation set up just yet.

SWIWS started out with a Performic and spent 3 weeks/$600 on chems n' sassy and for nothin' Tried the oxone and sucsess the first time! This was a lot of lab technique practice later and the amalgam is still tricky to get good yields. But hey it worked first time.
The Oxone route uses a shitload of methanol and dH2O but for the newbee the easy workup and easy aquisition of reagents make it a great choice (OTC). Even though the yields are about 35% less than other routes you are more likely to end up with fluffy yummy love powder at the end of the day. ;)  IMO anyways.

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

greeter

  • Guest
oops!
« Reply #10 on: June 10, 2002, 11:52:00 AM »
Sorry, didn't know to calculate molar yield.  Duh.  Will do in the future.

Thanks!

A watched pot will indeed boil.

aznxprophetxtasy

  • Guest
OK, i figured out overall i believe oxone to be ...
« Reply #11 on: June 10, 2002, 06:21:00 PM »
OK, i figured out overall i believe oxone to be easier and cheaper but does not have as good of yield here are my calculations...

For the  oxone route, reacting 50g iso-safrole --> epoxide requires (from my sources) $3.19 worth of chemicals and 5hours reaction time but requires a reaction flask of approx. 2L

For the performic route, reactiong 50g iso-safrole --> epoxide requires (from my sources) $5.10 worth of chemicals and 16hours of reaction time and only needs a reaction flask of less than 500mL.

So i figure the reaction with oxone may be better but which method produces cleaner epoxide??

Thanx bees for all the help so far.

aznxprophetxtasy

  • Guest
Oh yeah and... I care ALOT about the time it ...
« Reply #12 on: June 10, 2002, 06:24:00 PM »
Oh yeah and... I care ALOT about the time it takes to convert to epoxide, the oxone rxn is 3 times quicker so that helps me a bunch.

Chromic

  • Guest
Not correct!
« Reply #13 on: June 10, 2002, 09:43:00 PM »
The Oxone in MeOH takes LONGER than the peracetic in dcm or performic in dcm. Choose the oxone method only when you do not have access to other superior methods (ie benzo wacker due to its high cost and availability of reagents, performic due to availability of formic, peracetic due to availability of acetic, etc).

aznxprophetxtasy

  • Guest
hmm according to rhodiums site reaction for oxone ...
« Reply #14 on: June 10, 2002, 10:45:00 PM »
hmm according to rhodiums site reaction for oxone to convert to epoxide is roughly 5hours and the reaction for performic to convert iso-safrole to epxoide is 16hours with buffered performic. Am i mistaken somwhere?? and why is performic superior? Does it produce more pure epoxide than the oxone method?? SWIM need answers before SWIM goes out and buys the chemicals....

Chromic

  • Guest
Oh my goodness..
« Reply #15 on: June 10, 2002, 10:54:00 PM »
Uh, dude... I think you should do more research. You want ketone, which will mean that you have to take the epoxide from the persulfate method (oxone) and treat it with 15% H2SO4 just as in the performic and peracetic methods.

aznxprophetxtasy

  • Guest
ummmmmmmmmm K....
« Reply #16 on: June 11, 2002, 12:46:00 AM »
SWIM have done his research and SWIM plans to distill every step of the way. THAT means SWIM distilled his sassafras oil to get safrole, he then distilled that safrole again to obtain a purer fraction of safrole. Isomerized and distilled to collect two different fractions iso-safrole and safrole. Distilled the iso-safrole another time. SWIM wanted the best quality everything but doesnt like to distill because it takes forever, that is why i asked for the purity of epoxide so SWIM can skip the step of distilling epoxide. SWIM wants the highest yield (but he still wants it to be OTC) and the cleanest product possible. Because the purer your product the higher your yield will be when you do the reactions. Am I not correct?

As for the performic and oxone i was asking which produces a more pure epoxide so SWIM can just skip the step of distilling epoxide and just hydrolyze it with 15% H2SO4 to Ketone then distill the ketone straight. He dont want to go through the process of sodium bisulfite adduct if not necessary.

Thanks Chromic for all your help i think you were just mis-interpreting my question/knowledge. Yes SWIM knows the full process to make safrole--->MDMA.HCL by memory so you shouldnt doubt his knowledge.

I just want to have pure ketone without extra steps.

greeter

  • Guest
distilling epoxide
« Reply #17 on: June 11, 2002, 02:03:00 AM »
You don't need to do this.  Hydrolyse it then carefully vac distill the ketone.  Are you planning to distill your freebase as well?

A watched pot will indeed boil.

GlaseIs

  • Guest
Oxone vs Performic yield question
« Reply #18 on: June 11, 2002, 09:34:00 AM »
Hey just a quick question I have been wondering about but havn't seen the answer to: If both the performic and the oxone routes both yield glycol/epoxide in roughly 95% yields, then the only difference should be the hydrolysis. But the hydrolysis is the same in the two methods, then why are there such different yields in the two methods? Please could someone clear this up, it has confused me for the longest time. (Swim however is going the O2 wacker route w/ custom built reactor, clean, small, and easy imo)


On the 6th day God created man. On the 7th day, man returned the favor.

Rhodium

  • Guest
Chromic: How can you say the oxone route takes ...
« Reply #19 on: June 11, 2002, 12:43:00 PM »
Chromic: How can you say the oxone route takes longer time than the modified performic?

Have you done trial runs in shorter time with the modified performic and found that letting it react overnight is not necessary?