Author Topic: Safrole Isomerization via pentacarbonyliron  (Read 2204 times)

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b00ked

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Safrole Isomerization via pentacarbonyliron
« on: August 20, 2004, 02:55:00 PM »
Swim's previous attempt with this method worked however the vigorous reaction that was supposed to occur didn't. 2000ml of distilled safrole was placed in a 5L flask equipped with a thermometer and condenser. 10g Fe(CO)5 and 6.5g NaOH both ACS grade were then added. Solution immediatley took on a grennish/yellow color that turned a dark grennish/black color with heating. Solution was heated to 110 (no vigorous reaction) heating was continued up to 160 degrees. Resulting organic mixtures was distilled at 135-137 degress leaving a very slightly clear yellow oil. This was the only fraction to come over. When used in the performic it without a doubt produced MDP2P. Does anybody have any experience with this method? I know raflike did however it seems he is no longer part of the board. Swim is weary of using 15L safrole with this method, however, just KOH will take forever.

ApprenticeCook

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however, just KOH will take forever True but...
« Reply #1 on: August 21, 2004, 06:29:00 PM »
however, just KOH will take forever
True but how many people have access to pentacarbonyliron compared to KOH?
But it is another way to do something so thats always good, if you found an easy source for the pentacarbonyliron then everyone would bee much happier with this method.

What was your reference for this proceedure?
-AC


Saddam_Hussein

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underground
« Reply #2 on: August 22, 2004, 10:27:00 AM »

b00ked

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The procedure is from Rhodium's site.
« Reply #3 on: August 24, 2004, 01:06:00 PM »
The procedure is from Rhodium's site. At the bottom of the page the reference is there. The only problem with the method is when you wash with dilute acetic acid you encounter an almost impossible emulsion. Later attempts skipped this procedure all together.

b00ked

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Yes...I do have quite a habit, but admitting...
« Reply #4 on: August 24, 2004, 01:08:00 PM »