Vibrating_Lights (Hive Addict)
08-26-03 17:33
No 455856
      SYNTHESIS of 3Br-Methcathinone NAs assay  Bookmark   

All reagents were lab Grade including D-Ephedrine.

22 Gms Ephedrine Hcl was placed into a 1l RBf in a water bath.
A standard jones reagent was prepared.
.15 mole Jones reagent employed. This was added.  THe SOlution began to reflux it self after about an hour.  WHEN it slowed low heat was applied.  Reaction was followed with TLC to COompleteion.  6 Hrs.  The Rxn was allowed to coll and then was basified with SAturated KCO3. SOlution was vac filtered to remove percipitated Cromium. FIlter was washed with EtAcOH. THe FIlterate was extracted WIth  EtAcOH the FIlterates COmbined and solvent was removed on a rotovap.  Product verafied WIth NMR

Yeild 21gms D-Methcathinone

20 gms Methcathinone was DIssolved in 200Ml AA that contained .1M Bromine.
This was stirred FOr 4 Hrs. 

Rxn was basified and extracted into 200ml EtACOH.  This was washed with Na2SO4.  then BICarbonate.

THe EtAcOH was dried with NaSO4 and added to C.HCL iN acetone.
Yeild  17gms
3-Br-Methcathinone.  25-30MGS +++
NMR PIc Coming
COmments AND MANY MORE FUN HIGH POTENCY SYNTHS TO COME
LOve
Ya VL_

Start thinking more like a chemist and less like a criminal
 
 
 
 
    Vitus_Verdegast
(Hive Bee)
08-26-03 18:20
No 455864
      3-Br or 4-Br ??  Bookmark   

Question may sound abit stupid blushblush but...

Is bromination of methcathinone meta-directing because of it beta-carbonyl group, in other words does the 2-aminopropan-1-one sidechain deactivate the benzene ring?

I thought that activating groups generally win out over deactivating groups.

A Dream Within A Dream (http://www.poedecoder.com/Qrisse/works/dreamw.html)
 
 
 
 
    Vibrating_Lights
(Hive Addict)
08-26-03 18:53
No 455878
      yes  Bookmark   

yes.  the ketone deactivates the ring.  If you wanted to make 4 Br Methcathinone you would have to start by brominating the ephedrine FIrst then oxidise.
Http://www.geocities.com/axelfj/research.html

Start thinking more like a chemist and less like a criminal
 
 
 
 
    dennis_pro
(HyperLab Bee)
09-03-03 19:49
No 457105
      Are you sure?  Bookmark   

Are you sure that you've obtained a 3-Br-methcatinone? I'm think that bromine will attack near-ketone atom first, producing bromoketone (like bromacetone, for example), i.e. Ph-C(=O)-C(Br)(CH3)(NHCH3) or not? Did you make any analysis of your compound?

With best regards,
Dennis Prochko aka Wolf
 
 
 
 
    Blind_Angel
(Newbee)
09-03-03 20:49
No 457108
      Maybe a little of topic  Bookmark   

But, can someone explain me why adding a bromine on the 4th/3rd position of a ring make the honey more potent? (or refer me to a link)

/}/_//\//) /-|/\//¬/=/_
 
 
 
 
    hypo
(Hive Addict)
09-04-03 00:17
No 457136
      wtf???  Bookmark   

> But, can someone explain me why adding a bromine on the 4th/3rd position
> of a ring make the honey more potent? (or refer me to a link)

what the fuck are you talking about?? 2C-H? 2,5-DMA?

n'importe quoi
 
 
 
 
    Pimpo
(Stranger)
09-04-03 11:19
No 457187
      alpha bromo ketone VERY unstable  Bookmark   

Hi dennis_pro, indeed it would be a good idea to clearly establish the identity of the product. I just wanted to point out that the alpha-substitution product Ph-C(=O)-C(Br)(CH3)(NHCH3) you proposed would be highly unstable (bromo- and methylamino-groups on the same carbon). I guess it would eliminate HBr and form the imine Ph-C(=O)-C(CH3)(=NCH3), which again looks pretty unstable and might react to god knows what. I could imagine that A/B extraction does get rid of it, if it was formed. Just some speculation.