Author Topic: serious performic problems...shit  (Read 3180 times)

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b00ked

  • Guest
serious performic problems...shit
« on: August 04, 2004, 04:02:00 AM »
Hi guys this is my first post as a member, however, I've been lurking here for well almost two years. I have completed many synths and attribute all I know to this forum and Rhodium's page. Enough of the bullshit I've run into a snag. Here it goes.

5L of >95% sass oil was distilled between 120C -125C with 5 plate column. 2L safrole placed in 5L flask charged with 60g ACS grade KOH. Refluxed at 120C for 12hrs. Distilled with column to yeild >1900ml clear isosafrole. Smelled good. 1L weighed 1119g. 1300g isosafrole was placed in a 12L flask along with 3900ml DCM and 425g NaHCO3. Allowed to stir for 1hr. Performic acid made for 1.5L 35% ACS grade H2O2 and 2.5L 86% ACS grade HCOOH. Cooled to 0C before addition. Dripped in over 3hrs. Temp kept below 25C. Color turned for clear to exactly "orange juice" color. Allowed to stir for 14hrs. Deep orange DCM/glycol layer with clear top layer. Seperated in 6L funnel. OK here is where things got weird. As I began to strip of the DCM the solution turned a dark ruby red. I firgured over oxidation. I washed with 2x 700ml water and 2x 700ml 10% NaOH. Washes were dark blood red! Glycol didn't really clear up after layers seperated, only when mixing them did the Glycol layer turn its characteristic organge layer. Refluxed with 15% h2so4 to yeild weird red viscious oil that distilled into this yellow shit. Any ideas this is the second time this is bullshit. I've wasted over 3L of safrole. Help me out brothas.

Bandil

  • Guest
Save that yellow "shit"
« Reply #1 on: August 04, 2004, 10:48:00 AM »
That sounds pretty much like MDP2P to me?

So please don't throw it out. Try to do a bisulfite test on it to see if its the right thing you've got!

Regards
Bandil


GC_MS

  • Guest
MDMA
« Reply #2 on: August 04, 2004, 10:51:00 AM »
I've wasted over 3L of safrole. Help me out brothas.

Or you eat too much MDMA, or you must be an oversocial personality type.


ApprenticeCook

  • Guest
Oh this is a classic...
« Reply #3 on: August 04, 2004, 01:54:00 PM »
Oh this is a classic...
Theres:
I have completed many synths
Then...
yeild weird red viscious oil that distilled into this yellow shit

So when you get a synth that works you get the shits coz you honestly have no idea what the product looks like, although you have been lurking here for well almost two years oh my.....

Hope you have not thrown it out, otherwise you have thrown out heaps of money and heaps and heaps of shed 1 immediate precursor.... haha  ::)  :o  ;)

Ketone as decribed many tiems here comes out different colours every which way.... orange, yellow, red, blue (photo MDA synth on rhods has blue ketone!) talk about confusing! just ignore the colour after distillation and collect the clean distillate range correct for MDP2P.

And if you have thrown it out.... well.....  :(
-AC


b00ked

  • Guest
I've run many successful wackers and Al/Hg's...
« Reply #4 on: August 05, 2004, 06:02:00 PM »
I've run many  successful wackers and Al/Hg's before, however, only one performic before these attempts. Whether the reaction was a success is not the question I'm just wondering about the color change. Have any of you guys witnessed this and what effect does it have on the product? I know there is MDP2P in the flask It smells good but usually it has a lighter color. I will try bisulfate. Could there be an additive in one of the reagents I am using.

biffman

  • Guest
Surely you must be joking (Mister Feynman!)
« Reply #5 on: August 05, 2004, 09:49:00 PM »
Everything seems to be spot on in your write-up. (Well documented by the way).
 Except at the end where you start to panic for no apparent reason except that the color was slightly off as compared to your previous Wacker experiences.
  Unless you've tossed everything then should be a happy little camper and be doing a little happy dance right about now.
  BTW what was the final yield (in weight) of the final yellow stuff?

OcoteaCymbarum

  • Guest
Can over oxidation occur???
« Reply #6 on: August 06, 2004, 12:50:00 AM »
I was unaware it could happen.
Basically, if you leave it to stir for 24 hours its all fine. There's no over oxidation there.
After the hydrolysis, you get a dark red oil, which upon distillation turns yellow. Thats MDP2P. Better quality then the wacker. Wacker can give you neon green, I even heard orange and blue.
More side products occur in a wacker.
The ketone you got is probably just more pure then anything you've synthed before. A much cleaner distillation and a lot easier when doing the performic vs the wacker

b00ked

  • Guest
The reaction definately produced MDP2P, ...
« Reply #7 on: August 06, 2004, 01:06:00 AM »
The reaction definately produced MDP2P, however, I am just worried about the abrupt color change toward the end of the reaction. The previous performic yielded a clear mdp2p with the oldershaw column. This time is is dark yellow. Maybe my vacuum is on the brink. That baby has been through hell and back.

ApprenticeCook

  • Guest
The previous performic yielded a clear mdp2p...
« Reply #8 on: August 06, 2004, 04:00:00 AM »
The previous performic yielded a clear mdp2p with the oldershaw column. This time is is dark yellow.

Ignore colour, smell is sometimes misleading too. If it distills at the right temp for mdp2p and does the right rxn with bisulfite then your fine.
-AC


goiterjoe

  • Guest
sounds like the previous clear ketone was bunk
« Reply #9 on: August 06, 2004, 07:03:00 AM »
what you described is exactly what should happen, it you got clear ketone before, then it probably wasn't ketone but instead unreacted safrole.  The isomerization of safrole to isosafrole is the easiest step to fuck up, but also the hardest one to pinpoint as the problem.


b00ked

  • Guest
success...
« Reply #10 on: August 08, 2004, 11:56:00 PM »
Distillate formed bisulfate adduct. Awesome.  I will follow up on reductive amination results. Sauce is being stored in deep freeze now. Still no reply on possible theories or experiences on dark red finishing color of the performic. Anybody it's really becoming a thorn in my side.

ApprenticeCook

  • Guest
As i said before the results of colour are not
« Reply #11 on: August 09, 2004, 04:18:00 AM »
As i said before the results of colour are not reliable, dont worry about what colour it is... the colour of ketone varies on the method used to make it, and even then there is a fair amount of variance...
Personally i have had yellow, dark orange, light brown (sort of golden syrup colour), fluro yellow (that was cool!) and red.
I have never seen blue, but heres the link to the page with the picture, weird but is a good example of what i mean when i say its not reliable enough to work on colour of the ketone.

https://www.thevespiary.org/rhodium/Rhodium/clandestine/nasa/index.html


Ketone -->

https://www.thevespiary.org/rhodium/Rhodium/clandestine/nasa/ket2.jpg



-AC