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AMT from indole [pictures]
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brain
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re: AMT from indole [pictures]

 Sun May 29, 2005 3:19 pm		 Reply with quote
because its wery messy Smile if i can reduce this oil [orange crystals and oil solubled in small amount of IPA] i will add this solution to Al/Hg ... i will then try to clean final product - if the yelds will be the same- I THINK that puryfying sub-products in ewery step will be stupid ! because you hawe to clen final produdt to ! and in all steps there arnt formed any dangerous by-product in much quantytis that couldnt be separated in final puryfying ....

if i dont hawe to puryfy sub-products only final-product, then i could do all this steps in one day ! when puryfy-recrystalize, freez etc. then 3-4 days ...
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Re: re: AMT from indole [pictures]

 Sun May 29, 2005 4:27 pm		 Reply with quote
brain wrote:
I THINK that puryfying sub-products in ewery step will be stupid ! because you hawe to clen final produdt to !


In my experience, failing to purify reaction intermediates in these types of reactions will lead to substantially lower yields and sometimes the final product is even impossible to isolate because there are so many by-products. But by all means try it and report back......You may have more luck Smile
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brain
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re: AMT from indole [pictures]

 Sun May 29, 2005 6:40 pm		 Reply with quote
I'm sory synthetikal, i dont konw i will able to write writeup so quick, i hawe so many synthesis to do, and so little time Sad Wink

quite succesful day Smile reducing that dirty orange crystaline mass, and also mixture from condensation! widouth isolating crystals! [etno2, aldehyde]

I get CLEAR colorless oil ! i ewerycase, i just washed with Et2O - when it reduced and adding AcOH, than, add NaOH, and another wash with Et2O-that wash was sawed, and air dryed [ether ewaporate] now oil is in the freezer, i can se there are some cryslals formed - the crystals formed! mp-95C, this can be easly rised by recrystalization from ethyl acetate.

Al/Hg amalgam :


AcOH+IPA [i dropped to id little of crystals by accident-so color is yellow, its only 1-2 small crystals] :



adding Al/Hg to AcOH+IPA :


than i added slowely crystals, temp slowely ! rised 40C, weeeery slowely, not like in P2NP, after a while solution become dirty GREEN ! it sometimes happened in p2np :


Added some AcOH, and wash with Et2O (slight yellow solution) from what the nitrocompound can be recrycled Smile again used :


added NaOH and extracted with Et2O :


when Et2O was weaporating, whe solution becomes milky-white (crystals are formed, and oil separates form ether !! it can be seen!) :




some crystals are formed :
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Re: re: AMT from indole [pictures]

 Sun May 29, 2005 7:26 pm		 Reply with quote
brain wrote:
quite succesful day Smile reducing that dirty orange crystaline mass, and also mixture from condensation! widouth isolating crystals!


Well done. Al/Hg is obviously quite tolerant to impurities. I know if one were to take the nitropropene through a borohydride reduction and then Zn/HCOOH or reduce it using sodium bis-(methoxyethoxy) aluminium hydride then the yields would be pretty low without recrystallizing. Make sure that you report your yields after recrystallization - it would be really interesting.
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