Recovering Water Contaminated Fumarates in Xylene.

[polmos]

Fasa was added to the first xylene pull & there was virtually no clouding, only a lighter colored layer underneath the xylene-DMT layer. I have a strong feeling the acetone was contaminated with too much water...

How can this be recovered ???

 

[polmos]

Im guessing adding an ammount of FASW to it, then pulling the water layer, re-basing then pulling with xylene would do the job ?

 

[Du57mi73]

That would work. But if you added Fumaric Acid and nothing happened i would go to assume that you dont have anything in the xylene for the FA to react with OR there wasnt enough FA. If you know for a fact you had both of them then you might want to consider evaporating both the acetone and the xylene and starting over.

 

[downwardsfromzero]

Fasa was added to the first xylene pull & there was virtually no clouding, only a lighter colored layer underneath the xylene-DMT layer. I have a strong feeling the acetone was contaminated with too much water...

How can this be recovered ???

Did you dry your xylene extraction after separating from the basic aqueous phase? Anhydrous sodium carbonate would probably do the trick there.

Do you keep your FASA in a tightly stoppered container?

Was your acetone sufficiently dry in the first place?

FASA/xylene appears somewhat fraught with moisture sensitivities, IMO. Assuming the aim is to obtain crystalline fumarates directly.

 

[Bdevall158]

i had this problem once, i had all my crystals forming once the fasa was added, but stupidly i kept the container in my bathroom cabinet and after a good shower the high humidity made all crystals dissolve. i just added excess water and evap the xylene of then evap remaining water. fumarates are water soluble so the excess water wil pull them all out of the xylene