Hello, can you help me.
I use excess dibutyl phosphite to synthesize my starting organophosphorus compound
Is there a way to easily purify the compound from the phosphite in the reaction mixture?
It is possible with column chromatography, but in some cases the phosphite also comes out with the starting compound.
I tried vacuum distillation, but my compound also over distilled and also degraded a little when heated
Is it possible to wash out the phosphite and what should I add for this?
Thank you!
The simplest is oxidation or anchoring with electrophilic reagents. Oxidation with iodine I2 is a fairly mild method, in the presence of a base (soda, pyridine, N-methylimidazole) you will get a dibutyl phosphate salt, which can be washed off with water, it is also well sorbed on silica gel.
I added I2 and base to my mixture in water, then stirred. After extraction, the reaction mixture of course acquired a brown color, but according to GC, the phosphite content in the mixture actually decreased, although some new by-products appeared. Anyway, your answer helped me. Thank you, Andrei Rogoza!
Everything turned out to be much simpler. If we deprotonate the phosphite to bind it to the electrophilic agent, then we can simply transfer the anion form of the phosphite into water. I added water, ethyl acetate, tBuOK to my mixture and stirred it thoroughly. There was no phosphite in the organic phase at all. If your substance can withstand such a strong base as tBuOK, then the method is really effective.
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