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All 7 posts Subject: SYNTHESIS of 3Br-Methcathinone NAs assay Please login to post Down

Vibrating_Lights
(Hive Addict)
08-27-03 00:33
No 455856
      SYNTHESIS of 3Br-Methcathinone NAs assay

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)
08-27-03 01:20
No 455864
User Picture       3-Br or 4-Br ??

Question may sound abit stupid blush blush 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)
08-27-03 01:53
No 455878
      yes

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)
09-04-03 02:49
No 457105
User Picture       Are you sure?

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)
09-04-03 03:49
No 457108
      Maybe a little of topic

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 07:17
No 457136
      wtf???

> 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 18:19
No 457187
      alpha bromo ketone VERY unstable

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.

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	All 7 posts		Subject: SYNTHESIS of 3Br-Methcathinone NAs assay		Please login to post		Down


		Vibrating_Lights (Hive Addict) 08-27-03 00:33 No 455856				SYNTHESIS of 3Br-Methcathinone NAs assay
						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) 08-27-03 01:20 No 455864				3-Br or 4-Br ??
						Question may sound abit stupid 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) 08-27-03 01:53 No 455878				yes
						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) 09-04-03 02:49 No 457105				Are you sure?
						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) 09-04-03 03:49 No 457108				Maybe a little of topic
						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 07:17 No 457136				wtf???
						> 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 18:19 No 457187				alpha bromo ketone VERY unstable
						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.

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