hi,

I have a big problem ..
I'm dreaming of ketone from performic ...
The reaction runs fine .. until it's time to distill the ketone ..

My distilled this black, there are several colors in the condenser.
blue, red, green, purple, black ... very strange ..
and my ketone end this 100% black.
the vacuum distillation is happening to .. at a temperature of 178C

did 3 Reactions with 1200g glycol
I do the washes ..

pure water
NaCl
5% NaOH (4 liters washings made ??up to 8 liters)
I also wash with baking in another dream ..
then do another washing with NaCl
dry ..
distill ..

I already did wacker oxidation .. and it never happened ..

I do not idea what is going on ..
someone who etende of performic please help me?

thank you

probably to do with the purity of your safrole and the other reagents. Worst comes to worst just run it in a wacker oxidation with either benzoquinone or isopropyl nitrite. It is very difficult for people to deduce what the problem is on your end, let alone when your english is patchy and reagents arent referred to properly.

Purity of safrole
Purifty of other reagents

The problem will lie in the above two points unless you're not following the instructions.

It sounds as though your crude ketone boiled over and up into your still head and condenser. There is NO WAY it should be black or any colour other than slightly yellow/green. All the black should be left in the distillation flask, not in your receiver. You need to redistill this and pay attention the entire time.

Seal joints properly, start stirring, turn on vacuum, SLOWLY raise the heat, until it begins to boil, when temperature in your still head stabilizes discard the forerun, add new receiver flask, re apply vacuum being very careful it doesn't boil over. If it does boil over then you start all over again. Eventually the temperature in the still head will begin to drop, meaning the distillation is over, the remaining stuff in your flask is polymerized crap, get it out of you flask before it hardens and becomes impossible to remove.

Good luck, proper distillation takes patience.

You might want to read:

https://the-collective.ws/forum/index.php?topic=9873.0

before proceeding    The end results from the effort applied 

As posted above, you need to study:

https://the-collective.ws/forum/index.php?topic=9873.msg52790#msg52790

and

https://the-collective.ws/forum/index.php?topic=9873.msg52792#msg52792

for as long as it takes to understand what you're attempting to do    Your account was approved  after registration so all you have to do is log in and start reading There are several threads on this web site that you should read as well  The end results from the effort applied 

I dont know how big the batches are that you're running, but scale them down to below 50g of ketone per, preferably less. There is no point wasting valuable materials.

thanks for the advice.

in a new dream ..
1200g glycol washed with 10 liters of 10% NaOH (much)
then the pH was basic ..
dried ...
the first drops of yellow ketone were after was becoming darker colors ..
and then measured the pH was acid!

I do not understand ..
the pH was basic and transformed to acid during distillation?

someone please help me?

LT/ and Ritter stated:

The PerAcid solution is made from 25 g. HCOOH (formic acid)(86% ,starting from 99% HCOOH) and 15.1 g. 30% H2O2 (hydrogen peroxide).
This sol. is added to a mixed sol. of 16.25 g. Isosafrole(>/=90%) and 1,5 g. NaHCO3 (!!) in 50 ml CH2Cl-CH2Cl at 35-40 C.
The temp. is during 6 Hrs. mixing regularaly checked and kept within 35-40 C.
The solvent is evaporated (vacuum, keep TEMP! UNDER! 60 C.!).
Residue is boiled with 180 g. 15% H2SO4 for 2 Hrs.
Extraction with 3 x 100 ml.CHCl3, wash with water,dry over MgSO4 and evaporation of the solvent gives a brown oil (purity >/=90%).
Supplemental purifying by Kughelruhr destillation (~70 C, 0,2 Torr) gives 70-75% yield of MDP2P (>/= 95% pure!)

~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~

And this is the latest info from Ritter, who by the way posted this method first, then Beagle_boy , then me, then Gyrogearloose, so this method needed 3 times posting to get the attention needed, so lets call it from now on the Classic Performic, to avoid any misunderstandings:

Ritter
(Stranger)
06-20-00 14:26
Re: LabTop modified performic method?

The reaction runs best as described in my writeup! Adding carbonate to formic/peroxide first would surely lead to a nasty volcano and would not help any. Carbon Dioxide is emitted as performic is slowly added to alkene/carbonate solution. As far as advances are concerned a few things have been realized. Extremely vigourous stirring, such as that produced by a mechanical stirring rig, seems to increase yields. If a considerable amount of isoalkene is recovered during vacuum distillation an easy solution is to add more performic acid mix to rxn. This is usually an indicator that the peroxide used has degraded somewhat below 30%.
With this MDP2P you proceed to make :

in

https://the-collective.ws/forum/index.php?topic=9873.msg52790#msg52790

many members wash with brine instead of water    MDP2P can be steam distilled though it's very slow    It's clear that the study didn't result in comprehension    The end results from the effort applied 

Have you tried on a smaller scale?

There are numerous reactions that can occur in distillation leading to polymerization involving the methylenedioxy bridge    Your crude ketone isn't clean enough, you need to wash it more if you want to avoid the problems you're having    You haven't studied that thread enough apparently, perhaps it's going to take a few weeks of reading to comprehend what's been written     The advice to reduce your scale is clearly on point, you're a long ways from learning what you need to know