I tried by DCM and water wash but not getting compound in organic layer. Any suggestion or reference is much appreciated.
Evaporate it (11 mbar at 40 deg C) on the vacuum evaporator. Then pour in toluene and evaporate again. Repeat 2 or 3 times.
To remove DMF from a water-soluble compound, use vacuum rotary evaporation followed by aqueous dilution and extraction with diethyl ether or adsorption on resins. For high-MW compounds, dialysis is highly effective.
Wash the solution 2-3 times with fresh batches of Et2O then combine them. Dry them over MgSO4, filter and rotovap.
Two exotic variations: Azeotropes with
- 2,2,3,3-Tetra-Fluoro-propionic acid: at 20 Torr about 33 % DMF at a b.p. from 40 °C - or:
- 2,2,3,3-Tetra-fluoro-propionamide with about 34 % of DMF at a b.p. from 91 - 94 °C at 20 Torr.
More commonly:
Azeotrope with p-Xylene: 134 - 135 °C, normal pressure, with 18 % to 19 % DMF.
Mix with p-Xylene, distill of (first) p-Xylene-Water azeotrope, then add p-Xylene an do the azeotropic distillation until all DMF is removed. Your product is now in Xylene.
btw: DMF doesn't build an azeotrope with water ...
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