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Author Topic: Isomerization of safrole.  (Read 262 times)

thescientist3000

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Isomerization of safrole.
« on: November 18, 2011, 05:24:39 AM »
Is this a straight forward procedure?

heat saf to boiling, to ensure no moisture.  add KOH.  reflux under vacuum for 6-12 hours.  filter.  distill.  ?

He has heard of the KOH and CaO method as well, but this tends to leave a lot of sludge, and tar to filter/clean...although reflux time is down to a short 15 minutes!

Any tips or notes?

Thanks.
« Last Edit: November 18, 2011, 11:36:51 PM by thescientist3000 »

Vesp

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Re: Isomerization of safrole.
« Reply #1 on: November 18, 2011, 05:36:44 AM »
http://127.0.0.1/talk/index.php/topic,369.0.html

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Wizard X

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Re: Isomerization of safrole.
« Reply #2 on: November 18, 2011, 10:04:40 PM »
Quote from: thescientist3000 on November 18, 2011, 05:24:39 AM
Is this a straight forward procedure?

heat saf to boiling, to ensure no moisture.  add koh.  reflux under vacuum for 6-12 hours.  filter.  distill.  ?

I have heard of the koh and cao method as well, but this tends to leave a lot of sludge, and tar to filter/clean...although reflux time is down to a short 15 minutes!

thescientist3000: I assume you've looked at http://www.erowid.org/archive/rhodium/chemistry/isomerizafrole.html Ensure you vacuum distil the safrole from the sassafras oil first, before isomerization.
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thescientist3000

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Re: Isomerization of safrole.
« Reply #3 on: November 19, 2011, 01:19:02 AM »
hi wizard.

sas was distilled to yield saf.

saf was isomerized a couple ways which will be tested to see which method is best in the final product.

1. saf heated to boiling under vacuum. vac removed and KOH added.  vac added, and refluxed for 8 hours. filtered, and distilled to yield clear oil similar to starting oil saf.
2. saf heated to boiling under vacuum.  vac removed. KOH and CaO added.  vac added, refluxed for 1 hour, filtered, distilled oil.

isomerizing without vacuum is a waste. 

the procedure seems simple enough that it cant be messed up, so im wondering where all the secrets lie in this... it appears there is success tho.

lugh

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Re: Isomerization of safrole.
« Reply #4 on: November 19, 2011, 02:05:01 AM »
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Hawkwind

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Re: Isomerization of safrole.
« Reply #5 on: November 19, 2011, 04:21:19 AM »
Some have recommended steaming or distilling off the 15% water typically present in 85% KOH before reflux when using KOH alone, don't know if that might affect yields.

thescientist3000

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Re: Isomerization of safrole.
« Reply #6 on: November 19, 2011, 09:17:19 PM »
Hi Lugh and Hawkind.

I will hopefully be able to check that link out soon enough.

Hawkind- In the past a ferret has heated oil slightly, added KOH, and than vacuum.  Once vacuum was applied it bubbled slightly indicating moisture was being taken out.  This occurs for a couple minutes than settles.  Usually there isnt enough moisture to get any drops to come over...  Heat is then increased under vacuum until reflux... 

Sounds similar to what your saying.
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