Author Topic: Bromosafrole Made Easy  (Read 25048 times)

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Bwiti

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Bromosafrole Made Easy
« on: April 17, 2001, 04:24:00 PM »
Here's my idea: Add about 200g Na/K bromide to a 500ml flask, rig a 250ml sep funnel to the flask, which contains H2SO4. Have a tube leading from the flask to a large raft, and make sure everything's air-tight. Drip the H2SO4 into the flask and fill the raft with the HBr. Add a shit-load of safrole to another 500ml flask and add just enough acetic acid to dissolve the safrole. Put the flask in NaCl/ice, rig the raft up to it. Then put a 20 pound weight on top of the raft, which will speed-up the saturation of HBr. Let it be for about 2 days, let the acetic acid evaporate and you'll be left with a mean chunk of bromosafrole! My concern: Would anhydrous HBr eat through a rubber raft? Peace! :P


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yellowjacket

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Re: Bromosafrole Made Easy
« Reply #1 on: April 17, 2001, 08:45:00 PM »
Im confused. The raft does what now? where does it go in relation to the other stuff? And what is a raft?


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Bwiti

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Re: Bromosafrole Made Easy
« Reply #2 on: April 18, 2001, 12:35:00 AM »
"And what is a raft?"



 

 


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foxy2

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Re: Bromosafrole Made Easy
« Reply #3 on: April 18, 2001, 02:40:00 AM »
Why not pipe the HBr right into the safrole as its being made?
::)


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goiterjoe

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Re: Bromosafrole Made Easy
« Reply #4 on: April 18, 2001, 09:41:00 AM »
pipe the gas into a large hard plastic container(like a gas can) instead of a raft.  then pump a non polar solvent into the container to displace the gas and pressurize it.  I doubt that a raft would take but about 2atm of pressure to burst, and that cloud would do a number to your lungs and skin.



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Bwiti

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Re: Bromosafrole Made Easy
« Reply #5 on: April 18, 2001, 09:48:00 PM »
"Why not pipe the HBr right into the safrole as its being made?"

  I'm impatient - it takes too long to bubble HBr into safrole/acetic acid, so I figure that hooking-up an HBr-filled raft and putting weight on it will get the job done. The concentration of HBr definately would be enough to get good yields. I'm gonna search altavista to see if HBr is compatible with synthetic rubbers and similar materials. Peace! :P


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foxy2

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Re: Bromosafrole Made Easy
« Reply #6 on: April 18, 2001, 09:56:00 PM »
Well if you say so.

Look at it this way.
1.  You will have to babysit the acid (HBr) production if you use your infamous raft method.
2.  You will have to slowly bubble the HBr into the safrol/acetic

Why not just do both at the same time???
Ever hear of two birds with one stone?
:)


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improv_chem

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Re: Bromosafrole Made Easy
« Reply #7 on: April 19, 2001, 08:41:00 AM »
just one possible problem: will your HBr generator produce just HBr or will some Br2(g) be formed as well.  The Bromine might fuck up the process by making some di-bromosafrole.  There is a thread about this in chemistry discourse called HBr bubbly bubbly..
Is there any way to get rid of any bromine gas that might be in the HBr?

Happy Rafting! :)



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Bwiti

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Re: Bromosafrole Made Easy
« Reply #8 on: April 19, 2001, 09:06:00 AM »
"Is there any way to get rid of any bromine gas that might be in the HBr?"

  Add a little dH2O to the NaBr before starting the H2S04 drip?

"You will have to slowly bubble the HBr into the safrol/acetic"

  Hook-up an off/on valve between the HBr and flask. Or, I could just give-up on my raft idea.
:P


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goiterjoe

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Re: Bromosafrole Made Easy
« Reply #9 on: April 19, 2001, 09:29:00 AM »
IMHO, give up on the raft.  it sounds dangerous.  don't put a valve in the line either, as it will pressurize your gas vessel and might cause it to rupture.  just drip in the sulfuric when you want gas produced, using a sep funnel.


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Bwiti

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Re: Bromosafrole Made Easy
« Reply #10 on: April 20, 2001, 08:34:00 PM »
"just drip in the sulfuric when you want gas produced, using a sep funnel."

  In other words, keep it simple! Thanks and peace! :P


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Agent_Smith

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Re: Bromosafrole Made Easy
« Reply #11 on: April 21, 2001, 04:53:00 PM »
The NaBr and H2SO4 produces nearly all Br2, relatively little HBr:

NaBr (s) + H2SO4 (l)  HBr (g) + NaHSO4 (s)
2HBr (g) + H2SO4 (l)  Br2 (g) + SO2 (g) + 2H2O (l)

In SWIMs experimental procedures, even producing the gas in an ice water bath or with chilled acid results in load of Br2 and very little HBr (HBr is colorless but goes cloudy white on exposure to air, white wisps in red gas signify small amt.s of HBr in with Br2)

SWIMs other experiemnt was HCl + NaBr.  This resulted in an extremely small amount of redish gas (it looked yellow at low conc.), and a whole lot of gas that went cloudy white when hitting the air.  Just to check that this wasn't HCl gas, it didn't react with ammonia vapor.  SWIM is almost sure that this is HBr, chemistry chat rooms have agreed.

This gas was bubbled into sassy, which started out yellow and then went green progressing then into dark green.  Small amounts of red oil were viewed in splashes on the upper portion of the test tube, but the majority of the sol'n was dark green, almost black.  These color changes are nearly exactly what's to be expected when bromosafrole is made with KBr and DMSO.  Interesting, what do you think?  Also, see thread in chemistry forum "HBr bubbly bubbly"

PS, closer examination has revealed that the oil is indeed redish, but very very very dark, probably contanminated by gas generator, bubble-tube was stainless steel, but has given problems before.


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Bwiti

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Re: Bromosafrole Made Easy
« Reply #12 on: April 21, 2001, 10:35:00 PM »
"These color changes are nearly exactly what's to be expected when bromosafrole is made with KBr and DMSO.  Interesting, what do you think?"

  Damn! A while back, I was asking how one could make their own bromine, and the answers were more complex than just adding H2SO4 to KBr/NaBr. Are you sure about that? I've heard that the production of bromine can be avoided, and HBr produced by slowly adding the H2SO4 to a chunk of NaBr that has been moistened with a little H2O?
  When H2SO4 is added to KBr and DMSO, HBr is produced. <-- Everything in that procedure is anhydrous, so why can't I get the same results by adding H2SO4 to a dry bromide?
  Your HCl + bromide idea sounds good to me. Some excess HCl would probably end-up being mixed with the safrole. I wouldn't worry about that, because it's very hard to get HCl to react with safrole..The HBr would get the job done way before the HCl. What does everyone else think? Peace!  8)


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Agent_Smith

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Re: Bromosafrole Made Easy
« Reply #13 on: April 21, 2001, 11:02:00 PM »
R.e. the color changes, I was refering to the color changes decsribed when bromosassy is made via the frozen DMSO method with KBr, I was trying to show that the gassing was indeed producing the bromo safrole.

About the Br2, I tried H2SO4 and NaBr (anhydrous or nearly) once cold and once at room temp.  Each time copious amounts of Br2 was produced.  The mechanism for this Br2 production was found at

http://www.webelements.com/webelements/elements/text/Br/key.html


It states there that the "reaction conditions" oxidize the HBr to Br2, however it fails to elbarote on which conditions cause this, and it appears that chilled or not chilled had no effect.
Perhaps you are right about using moist NaBr and H2SO4, however I tried moist NaBr once and I saw the characteristic orange creep beginnig so I trashed it before it got going.

Youre indeed right about the HCl in the HBr made from NaBr and HCl.  I don't think the amount of HCl is all that large.  Then again it makes no difference, even if it did react, chlorosafrole would probably behave in the same manner as bromo so it's not a problem.


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Rhodium

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Re: Bromosafrole Made Easy
« Reply #14 on: April 22, 2001, 08:57:00 AM »
Both HBr and HCl will react with ammonia gas, forming ammonium chloride or ammonium bromide. If you didn't get any reaction, then your gas is not HBr or HCl, but something else.


http://rhodium.lycaeum.org


Agent_Smith

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Re: Bromosafrole Made Easy
« Reply #15 on: April 22, 2001, 09:43:00 AM »
Oh, I'll generate some more and test it with the ammonia again, never really liked that test anyway.


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Bwiti

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Re: Bromosafrole Made Easy
« Reply #16 on: April 22, 2001, 06:26:00 PM »
"About the Br2, I tried H2SO4 and NaBr (anhydrous or nearly) once cold and once at room temp.  Each time copious amounts of Br2 was produced."

  Damn, thanks man! In my dreams, you saved me from a big-time failure. Peace! 8)


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terbium

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Re: Bromosafrole Made Easy
« Reply #17 on: April 22, 2001, 09:22:00 PM »

The NaBr and H2SO4 produces nearly all Br2, relatively little HBr:

NaBr (s) + H2SO4 (l)  HBr (g) + NaHSO4 (s)
2HBr (g) + H2SO4 (l)  Br2 (g) + SO2 (g) + 2H2O (l)

In SWIMs experimental procedures, even producing the gas in an ice water bath or with chilled acid results in load of Br2 and very little HBr (HBr is colorless but goes cloudy white on exposure to air, white wisps in red gas signify small amt.s of HBr in with Br2)


But you weren't using pure NaBr. You were using a mixture of NaBr and an oxidizing agent whose purpose in the mixture is to oxidize the bromide to bromine.

Post 185107 (missing)

(Agent_Smith: "Re: HBr bubbly bubbly", Chemistry Discourse)


terbium

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Re: Bromosafrole Made Easy
« Reply #18 on: April 22, 2001, 09:35:00 PM »

"About the Br2, I tried H2SO4 and NaBr (anhydrous or nearly) once cold and once at room temp.  Each time copious amounts of Br2 was produced."

  Damn, thanks man! In my dreams, you saved me from a big-time failure. Peace!


Actually, Agent_Smith is throwing you a bit of a red herring by leaving out important experimental information - namely that he doesn't have pure NaBr but a mixture containing an oxidizing agent.

Post 185107 (missing)

(Agent_Smith: "Re: HBr bubbly bubbly", Chemistry Discourse)

Vogel prepares hydrobromic acid from from KBr and sulphuric acid. For anhydrous HBr he uses direct combination of the elements or the action of bromine on tetrahydronaphthalene.


goiterjoe

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Re: Bromosafrole Made Easy
« Reply #19 on: April 22, 2001, 09:59:00 PM »
wont the sulfuric + KBr produce anhydrous HBr if it works as said?


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