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All 5 posts Subject: Safrole Isomerization via pentacarbonyliron Please login to post Down

b00ked
(Stranger)
08-20-04 21:55
No 526521
      Safrole Isomerization via pentacarbonyliron

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
(Hive Addict)
08-22-04 01:29
No 526667
      however, just KOH will take forever True but...

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

Its just my opinion, but no-one listens to me anyway, and rightly so...

Saddam_Hussein
08-22-04 17:27
      underground
(Rated as: off-topic)

b00ked
(Stranger)
08-24-04 20:06
No 527120
      The procedure is from Rhodium's site.

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
08-24-04 20:08
      Yes...I do have quite a habit, but admitting...
(Rated as: off-topic)

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	All 5 posts		Subject: Safrole Isomerization via pentacarbonyliron		Please login to post		Down


		b00ked (Stranger) 08-20-04 21:55 No 526521				Safrole Isomerization via pentacarbonyliron
						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 (Hive Addict) 08-22-04 01:29 No 526667				however, just KOH will take forever True but...
						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 Its just my opinion, but no-one listens to me anyway, and rightly so...



		Saddam_Hussein 08-22-04 17:27				underground (Rated as: off-topic)



		b00ked (Stranger) 08-24-04 20:06 No 527120				The procedure is from Rhodium's site.
						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 08-24-04 20:08				Yes...I do have quite a habit, but admitting... (Rated as: off-topic)

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