Author Topic: Testing Isosafrole (w/o b.p)  (Read 611 times)

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amine

  • Guest
Testing Isosafrole (w/o b.p)
« on: February 17, 2004, 04:03:00 PM »
Swim is wondering if there is a way to test for isosafrole that does not involve heating it to 232C. Currently swim only has peanut oil which smoking point, I am sure is less that that of safrole.

Swim took 1000ml  of essential oil and added 100g of KOH to the solution, it was set up as if I were doing a distillation, temperature reached around 150C and stayed there for ~18 hours, the solution was a brown-dark brown color throughout the reaction, (iso)safrole was distilled via atmospheric pressure. Smell was different--similar to safrole but less 'potent'. 

A crude density test gave 1.10. Swim does not have access to tlc plates or a GC :(

Bandil

  • Guest
Not coherent statements mate!
« Reply #1 on: February 18, 2004, 12:29:00 AM »

Swim is wondering if there is a way to test for isosafrole that does not involve heating it to 232C.





(iso)safrole was distilled via atmospheric pressure. Smell was different--similar to safrole but less 'potent'




How did you distill it at atmospheric pressure without heating it to 232 degress if i may ask? If you have some sort of vacuum gaze, i'd love to learn your tricks  8)

The smell sounds about right, but it's no guarantee that it is isosafrole you have. Sassafras oil is usually more pungent than pure safrole, so that could be the answer.

But generally the isomerations are very hard to fuck up, so you've most likely got the right stuff! It's quite an amount of KOH you used. 1-2% usually ssufficient; 10% is waaay overkill!

Good luck.

Regards
Bandil




amine

  • Guest
my bad.... the iso was distilled under vacuum.
« Reply #2 on: February 18, 2004, 08:12:00 AM »
my bad....
the iso was distilled under vacuum.

I have some oxone laying around, so I'm thinking of running a small test this weekend and seeing if I do get ketone. Next time, I will use less KOH.

Zamboni

  • Guest
Melting/freezing point
« Reply #3 on: February 18, 2004, 07:24:00 PM »
Melting/freezing point

amine

  • Guest
Oxone will tell.....
« Reply #4 on: February 18, 2004, 08:05:00 PM »
Currently running the oxone with 30g of (iso?)safrole.

T+2hr10min. Reaction turned from a white solution to a yellow solution. Stirring is on.

From reading the noted by psychokitty the 1-alkene safrole shouldn't not react. So may be all is well.

btw, can the epoxide be xtracted with toluene? swim currently does not have any dcm on hand.

Antibody2

  • Guest
pseudonitrosite my friend
« Reply #5 on: February 19, 2004, 07:31:00 AM »
do a test tube scale pseudonitrosite rxn to test your iso.

put 5mls of saturated aqueous NaNO2 in a test tube
followed by 1ml of iso disolved in 20mls of pet ether

this will be biphasic

add a few mls 31% HCl or 25% H2SO4 dropwise (outside) there will be some red NO and NO2 fumes evolve, wait an hour or two and if you have iso you will see a cake of off white crunchy pseudonitrosite crystals floating on top of the ether

works like a charm 8)


amine

  • Guest
just tried the pseudonitrosite test, thanks...
« Reply #6 on: February 19, 2004, 08:40:00 PM »
just tried the pseudonitrosite  test, thanks for the help, distilled off the epoxide, color seems right, doesn't have much of a smell, (definitely not safrole).

Currently attempting the hydrolysis, acid is very dirty (drain cleaner) will have to look at purchasing a better cleaner acid later on. (Just making sure I got isosafrole)
;)