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Bromosafrole-DMSO WTF???

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somniferous:
Okay,

There's a lot of contradictory information re. the DMSO route to bromosafrole. Half of the posters claim success with this method, half claim it's garbage. The precursors are SO readily available that SWIM had to try...

500ml DMSO was chilled(Frozen solid is more like it) and 39ml chilled conc. H2SO4 was added. It warmed up a little. To this was added 150g NaBr. Turned orange. hmm.... Welp, in for a penny, in for a pound. And in goes 30g washed sassafras oil, slowly... stirred, stirred stirred, orange color disappears. Can't help but think I'm making di-bromo, f*ck it. stir,stir,stir... let sit cold for 36 hours... cloudy as heck from all the salts, but getting slowly darker...
For kicks, I open the jar, phew, smells like commercial propane, yuck. 50 ml of the reaction contents are removed and 300 ml of ice cold dH2O is added, within minutes a little bit of gloppy cloudy yellowish liquid falls to the bottom. Now at this point, if I listen to strangelove, I'm doing great. But it' not red. I don't like that. I like pretty colors...

So, a few questions-
Most of the failures reported were with KBr, not NaBr. This makes sense, KBr would probably produce more Br2. Could stricter temperature control increase the amount of HBr produced/reduce Br2 formation when using NaBr?

Strangelove swears by H2SO4+2NaBr in DMSO gives HBr and Na2SO4. Others claim the HBr is destroyed by the H2SO4 to give water and Br2. One reaction would give us our bromosaf, the other seems to produce a di-bromo-saf. The product strangelove described(and SWIM has) sounds more like the di-bromo(yellow, cloudy, not red at all). However, he claims success getting MDA from this stuff? Is this possible? Or more specifically:  Did he actually make bromo? Or, could the Di-Bromo-Safrole reported by some from the DMSO method be converted to MDA/MDMA within the bomb via an unexplored reaction? Or, I may  :(  have some experimentation data to share along this route soon as I figure out what the heck the cloudy yellow liquid is in the bottom of SWIM's snapple , um, reaction container.

At any rate, any feedback from someone with empirical experience would be wonderful, TIA.

Strung by a thin white hot wire,
burning with ecstacy

somniferous:
Okay,

After the full 48 hours had elapsed, 4l cold dH2O was added, and a tan milky fluid fell to the bottom. So far, it looks like I've made Di-Bromo...
To this some methanol is added. After stirring, the methanol turns a deep purple(yes, like the band  ;) ). So it looks like I made some bromosaf. The off white layer has lost some volume and is now white!!! It looks like it's at the lower end of it's liquid phase, so I warm some up(90C). It turns clear and darker brown. I let it cool and it whitens up, hmm.... no thermal breakdown yet. Seems like a homogeneous substance. I suspect it's Di-Bromo-Saf.

Since I don't have bromosaf(except maybe 5%-10% in methanol) I decide to play with my suspected Di-Bromo. I Heat some to 100C and it starts to bubble. I set up to distil, and get a dark brown-red, clear liquid. As I do this the alleged Di-Bromo Starts to darken. I let it cool, and it's greyish-white. Looks like some carbon is forming, thermal breakdown... Looks like I did make Di-Bromo!
That would make my dark brown liquid the 2,Bromo-propene. Whee!

So, Here's my thoughts-
1. The DMSO route to bromosaf is finicky, The reaction's main product was Di-BromoSafrole, not the desired 2,Bromo. Some 2,Bromo was formed. But not a lot... If I had to guess where it went goofy, I'd say batch size too large and not enough tempature control.

2. The DMSO/Bromo method to MDA/MDMA may be misunderstood. Hint, most reported failures used the Delepine rxn, not the bomb. Hint#2-Thermal Breakdown... I suspect the DMSO-H2SO4-NaBR method is valid(Flamebait, I know), but does not proceed as most think. Look for a post soon in the novel forum...  But, first, back to the kitch.  er lab. ;)

Strung by a thin white hot wire,
burning with ecstacy

somniferous:
Thanks,
If I dream that I'll probably bubble it through DMSO due to availability(farm country :) ). What I'm really trying to do is make sense of the H2SO4-NaBr thing and either prove or disprove the method(to myself at least). Even if I get nothing but garbage, I'll probably go at it again. I'm not really trying for product, just for knowledge. Acquiring the precursors is so ridiculously easy that even at 30% yield after amination, it would be economical. Plus, I suspect that people have actually made MDMA from Di-Bromo without realizing it, via the bomb. I've posted my idea over on the novel forum...

As far as making Bromosafrole via NaBr+H2SO4 in DMSO. I didn't make it work. But next time I'll be trying for Di-Bromo. (o.k.- I lied, I'm still trying for Bromosaf ;) )

Strung by a thin white hot wire,
burning with ecstacy

somniferous:
Well,
I'm back with another update.

Just tried to confirm my earlier suspicions about H2SO4+NaBr in DMSO.
Let me tell you about the dream I had-
60ml DMSO was frozen in a test tube. To this was added 4ml H2SO4. The DMSO immediately unfroze, and was chilled in Brine and ice for 15 min. Then 15g NaBr was added. No orange was evident upon addition of the NaBr! The Solids settled to the bottom and turned a light green. The DMSO remained absolutely clear. 2.5g safrole was added dropwise over 10 minutes. The solution remained clear and cool. About two hours have elapsed and it's starting to turn green! :)  So far, so good...

Conclusion- Scale and temperature seem to be the key components with this reaction. Small and cold is the rule.(The first try, the DMSO/H2SO4 was well below 75°C but formation of Br2 was evident. The guidlines for aqueous HBr production don't seem to follow with DMSO. If you add the NaBr, and see orange, cool it off some more.)

I'll post the complete results of the dream in 48 hours. Same Bat Time, Same Bat Channel.

p.s.- Thanks to everyone here! I've found this site invaluable.

Strung by a thin white hot wire,
burning with ecstacy

LaBTop:
That's a fine example of independent, logical thinking, and then checking your thoughts on nanoscale, and not spoiling gram- to kgmoles on not fully understood reactions. Waiting for the final test of the endproduct, LT.
Well done! New name: TestTubby! :)

WISDOMwillWIN

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