Hi all. I have been using diphenyl ether as the solvent for my cyclization reaction. I would like to know how to remove diphenyl ether from the reaction mixture (about 3-4 mL), and my compound seems to be dissolved in hexane.
Does the diphenyl ether not precipitate when you add hexanes?
Also why are you using diphenyl ether? What temp. is the reaction run at?
Sorry I was thinking of di-tert butyl ether when I asked the precipitation question.
I run the reaction at 250oC, normally my product will precipitate when added hexane, but in this time, it seems to dissolve in hexane, so I think about running the column. However, I don't know how to remove diphenyl ether?
You could perhaps consider to crystallize diphenyl ether from cooled hexane, to which chloroform and/or seeding diphenyl ether crystals could possibly be added.
first you check the TLC run hexane only how many spot is there first identified then all spot visible means you pack the column to high silica gel level slowly you can run the column it is possible ,otherwise diphenyl ether spot not visible means i given above procedure you can use but you should take run the column more time after put the %solvent it will easily separate.but you pack the column before full dry condition your compound with silica gel very important.
Dear Friend
1. Add co solvent to precipitate your compound by cooling to 0-5 0C.
2. OR Remove the diphenyl ether by high vacuum distillation.
Regards
Senthil Periyasamy
Perhaps you might want to try quinoline which is also a high boiling solvent but decent water solubility and could be extracted out
You might first cooled Rx mass to low temperature as melting point of diphenyl ether is 25 degree.In another flask cooled hexane to zero degree and then added to it stirred Rx mass and Decant hexane.
But as you mentioned this time your compound not crystallise this means you used Rx of low amount or may be impuritiy formed.
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