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safrole->MDP-2-P
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capacitor
unregistered posted 07-09-98 05:31 AM
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In a dream last night a person distilled sassafras oil and collected the safrole at a temp of 230 deg c.they then made isosafrole at 243 deg c.they then diluted 19.2ml of 50% H2O2 with 12.8 H2O added this to 141.2ml of 85% HCOOH with 8.8 ml H2O and the required isosafrole and acetone.the solution was kept at 22 deg c whilst mixed.the question I have is after 8 hr of stirring and the solution is still dark yellow and the temp is still at 22 deg c.is something going wrong here?
Osmium
Member posted 07-09-98 08:32 AM
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Cooling too much will stop the reaction. Let it react at approx. 30°C during the addition of isosafrole.
The acetone can be omitted (or at least reduced considerably).
You don't have to dilute your reaction with water. When you have stronger reagents, use them. They will work just as good or even better.
quirks
Member posted 07-09-98 06:41 PM
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With small amounts like that you might of acidently added too much water to the rxn. 50% H2O2 is ~4/3 as heavy as water. 19.2 mls is ~25 grams. Opps!!
If the soloutions too orange gentle warming in water seems to push it over the hump and it'll gradually turn a deep red.
The other day someone who was not me was distilling precious md-p2p and there was only a little bit of tar left in the flask and it was starting to smoke but it was still coming over and god damn if he was going to stop before every last drop was over, anyways all of a sudden it went POOF and filled the top 1/3 of his condensor, the coloum and the flask with this fucked up plastic-black-glass stuff. Far, far more of it then the volume of tar that was in the flask. wtf is up with that???
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