Author Topic: Test for Isosafrole...  (Read 1688 times)

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Semtexium

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Test for Isosafrole...
« on: September 19, 2001, 02:39:00 PM »
I KNOW I've read it somewhere but I cannot find it, it's pissing me off.  Does anyone remember a test for isosaf that had to do with a shot glass full of ice cold H2SO4...?  If so I'd really appreciate a copy of said test.  Or any other ways of determining iso from saf, yes I know about the different boiling points...  :P

::)  ;D  :)  :P  ;)     Mean People Suck     ;)  :P  :)  ;D  ::)

abc123

  • Guest
Re: Test for Isosafrole...
« Reply #1 on: September 19, 2001, 05:57:00 PM »
there is another way I have heard of...go to newbee forum and go back to 9/5/01 (about 150posts) and read the post from abc123. i think it is osmium that answers the question it is given in the last reply

abc123

goiterjoe

  • Guest
Re: Test for Isosafrole...
« Reply #2 on: September 19, 2001, 09:28:00 PM »
I remember there being an article in the erowid vaults about a guy who used a well known testing method to determine if he had safrole or isosafrole before proceeding with his experiments., and the test failed for him and the British version of the DEA that busted him.

Sed quis custodiet ipsos custodes?

Antibody2

  • Guest
Re: Test for Isosafrole...
« Reply #3 on: September 20, 2001, 06:22:00 AM »
Semtex, i beleive the method you refer to is for allybenzenes, and it converts the to an alcohol.

BUT!
a small scale pseudonitrosite rxn is exactly what you are looking for, i'll post details after i get the wife to work. It works like a charm, every time

"All those memories lost like rain..."

Chromic

  • Guest
Re: Test for Isosafrole...
« Reply #4 on: September 20, 2001, 09:09:00 AM »
TLC, index of refraction, boiling points, epoxidation/hydrolysis/bisulfite test. The first two assume you've got known isosafrole/safrole to test against. What's wrong with a BP test? Just put it in a flask with a condenser, and heat it up?

Antibody2

  • Guest
Re: Test for Isosafrole...
« Reply #5 on: September 20, 2001, 02:01:00 PM »
chromic, i've never heard of a bisulfite test for isosafrole, sure you are not refering to the ketone test?

semtex: anyways take a small arbitrary amount of iso, dissolve it in 10 volumes Et2O, dissolve 5 molar equivalents NaNO2, in the minimum amount of water reqd,  add 2.5 molar equivalents of 20-25% H2SO4. you should see a yellowing of the etherial layer followed by precipitate at the H2O/Et2O interface after 2-3 hours, works every time.

N.B. iso-myristicin and iso-apiole behave differently due to a pseudonitrosite that prefers to oil out :( , it will work but the work-up is exhauting.

But for isosaf this IS the shit, do it after every isomerization (just to be sure) :)

hope that helps

"All those memories lost like rain..."

Chromic

  • Guest
Re: Test for Isosafrole...
« Reply #6 on: September 21, 2001, 10:14:00 AM »
I was just saying that you react it, and test for the ketone.  :)

The only quick test I know of is adding a drop of isosafrole/safrole to a drop of sulfuric acid and checking for a burgandy color change.

The easiest way tho is to react with KOH and then distill at atmospheric pressure, watching the thermometer to check the BP. Then apply vacuum so you have an idea of what temperature your ketone will come over at.

baalchemist

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Re: Test for Isosafrole...
« Reply #7 on: September 22, 2001, 02:05:00 AM »
Test the S.D. before and after, that works well and is reasonably accurate.

GODISNOWHERE

LaBTop

  • Guest
Re: Test for Isosafrole...
« Reply #8 on: September 22, 2001, 05:47:00 AM »
Off topic, but Baal, how many would have seen the duality in your "GODISNOWHERE", never saw anybody mention it. GODISNOW HERE, GODIS NOWHERE.  Appropriate time to mention it, imho. LT/

WISDOMwillWIN

baalchemist

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Re: Test for Isosafrole...
« Reply #9 on: September 27, 2001, 06:02:00 AM »
LT; Your the first to pick up on it so far 

GODISNOWHERE

Vibrating_Lights

  • Guest
Re: Test for Isosafrole...
« Reply #10 on: September 30, 2001, 10:42:00 AM »
Swim drempt that a koh isomerization had failed because of cl contamination in the koh. He tested the suspected iso with a small nitrosaturation that yeileded a black and orange ball of polymerized crap that smelled like the saforle.

Antibody2

  • Guest
Re: Test for Isosafrole...
« Reply #11 on: October 01, 2001, 09:55:00 AM »
vibrating light - if it was an allybenzene, i do not beleive it would form any sort of solid, rather it would remain dissolved in the ether layer.

the fact that a solid precipitated from the etherial layer, indicates that a rxn took place. from the sounds of it, solvent may be to blame for polymerized gook product. what solvent was used & was it pure? OR it may be the isosafrole had contaminates.

a further check would be to see how that ball of crap fares during hydrolysis, the 10% KOH ethanolic hydrolysis solution, should dissolve the crud just fine leaving a yellow snow storm in an ugly looking hydrolysis mixture.

the precipitate from a successful nitrosation should be white to very pale yellow crunchy granules.


"All those memories lost like rain..."

goiterjoe

  • Guest
Re: Test for Isosafrole...
« Reply #12 on: October 01, 2001, 03:50:00 PM »
I can't find anything on the net about Fiegel's Spot Test, which is what I made reference to earlier over at the erowid vaults.  However, this story sounds more like a coverup for a mob-run exstacy lab to keep the guy out of jail.

Sed quis custodiet ipsos custodes?