If any of you are familiar with the fentanyl synthesis by Seigried from Rhodium, it mentions other seperation techniques would be required if you had para-fluro-fentanyl by using para-fluoro-aniline. Would anyone have any ideas as to what would be required to separate this? What about if you have para-chloro-alpha-methyl-fentanyl? What method would have to be modified assuming you got to the point of having the PCAMF? Is this insoluble in methylene chloride?
Also, in his method he states "When all the Propionyl Chloride is added, the reaction mixture is stirred for about one hour at room temperature.
Check the conversion with any method and if not complete, add another 1 mmol of Propionyl Chloride. Normally the conversion should be complete after the first operation but if there is too much Aniline you need more Propionyl Chloride."
What would be a good way to see if conversion is complete?
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