cheeseboy (cheese head)
03-12-02 12:05
No 281187
      Buffered Oxone  Bookmark   

Cheese has success getting ketone from Isosafrole but weak yields (first time ever)/ The first rxn was buffered with sodium bicarb. the epoxide oil was found in dark red globules at the bottom of the beaker. The second time was scaled down half as much and followed advice not to buffer the solution with bicarb cause it aint neede. Well needless to say, after extracting the epoxide from the mix with toluene, the toluene was stripped off and cheese was hoping it would look the same as before (green oil) but after the toluen was evapped, the brown oil just started smoking and tarring up, it smelled like a smokey cheescake gone rotten. Harsh smokey smell, never the less, this oil wouldn't distill, so I said fuck it. Where did Cheesboy go wrong this time. have a funny feeling that constant slow addition of sodium bicarb is the only way to go....anyone care to emulate on the disater (learning experoence)

Just pray that thew first 30gm of pale yellowish green oil will aminate alkright. let you know in 24 hours, Good night

Cheeseboy-a whiteboy with Soul Like a black guy without soul
May The Source Bee With You Always.
 
 
 
 
    LaBTop
(Daddy)
03-12-02 12:28
No 281205
      Re: Buffered Oxone  Bookmark   

A perfect example how a labreport should NOT look. Can't do anything with these words.
Too much to mention what is missing all there. LT/

WISDOMwillWIN
 
 
 
 
    cheeseboy
(cheese head)
03-12-02 20:35
No 281372
      Re: Buffered Oxone  Bookmark   

GROGGY!!!!SORRY DADDY: (the clonazepam was hitting hard as I wrote that last post)
Introduction:  last night there was something that went wrong with cheese's oil/epoxide. Let's figure out what is was!
  
Procedure:
       Epoxidation of isosafrole via Oxone solution in methanol/dH2O.

Reagents:
 
     1.  100gm Isosafrole
     2.  1000ml meoh
     3.   2800 mls dH2O
     4.   400gm Oxone
     5.   150 gm Sodium Bicarbonate added at the end of the 6 hour spin.

  The first run cheese tried was double this, the sodium bicarbonate was added slowly throughout the  rxn, and the epoxide/ glycol turned out to be sinking on the bottom of the aqueous layer as a dark red oil.The mix was rather warm (not RT) This oil was refluxed with 15% H2SO4 but 2 layers foremd so cheese just shook it like a mad man then the oil was converted to ketone via thermal rearrangment. Good to Go.

  The second attempt was scaled down 1/2 size and when the 6 hour spin was up then the bicarb was added slowly, the mix was at room temperature, not hot like the first batch. BUT there was no red globs of oil sitting on the bottom of the aqueous layer.

   The whole aqueous layer was extrated with toluene like the 1st run and the toluene went dark yellow/orange. After stripping off the toluene the temperature climed to 120C from 80C and then the black goop started smoking in the flask and smelled like a bacon burning smoke fest.The H2SO$ treatment wasn't applied since they say you can do without it, but since cheese never added buffer, the glycol was formed and was thermally rearranged w/o an acid wash first (THERE"S THE PROBLEM!!)Cheese noticed that the acidic oil was wrecked upon a thermal rearrangement Not fun, very stinky and messy shit. The stir bar was stuck so hard in the bottom of that crud it took 1hr of acid treatments to get it out and it sttunk bady. Why did the second run fail compared to the 1st run? The only thing cheese can think of is that there was a leak in his vacuum hose and the glycol got too hot and burned.But NOW cheese knows that the buffer bicarb MUST be added if the oil is to be thermally rearrangmed w/o an acid treatment first. Cheese smelled the exact same smell when he burned his epoxide the VERY FIRST time(a long time ago) trying this run using 2 gm of Iso (nana for fun). Has anyone ever seen this tar shit form from this procedure?

Conclusion:  Buffer the Oxone solution with sodium bicarb from start to finish, not just at the end, this will yield the epoxide, therefore being able to convert to ketone from thermal rearrangment. Maybe the H2SO4 is neccessary as well??? Back to the 'ol drawing board.
 LabTOP: Sorry for wasting your time with 1st thread, thanks for not closing this thread up. Tonite we will see if the yellow/green ketone that smells like,burned flowery medicine (unlike the lab grad ketone obtained through a chinese firm, which was more creamy smelling and more like the sassy smell, bright yellow/hint of green) The ketone was cleaned up nicely using sodium bicarbonate washes, which turned the water wash pink and left the ketone a more yellow than green. Luckily cheese only had barely enough ammonium acetate to aminate the 30gm of ketone so, it's all good anyways. Just need to figure out what went wrong with the tar smokiness crud that was a terrible smokey smell. Like a smoked hot dog or something. Kinda like burned meat.???hehe wierd but shitty as well eh?!  Well LabTOP, do you have any ideas now?

Cheeseboy-a whiteboy with Soul Like a black guy without soul
May The Source Bee With You Always.