Liquid-liquid extraction of DMF

A method for the chlorination of a sucrose-6-acylate to produce a 4,1,6-trichloro-4,1,6-trideoxy-galactosucrose-6-acylate wherein said method comprises: (i) combining the sucrose-6-acylate with a chlorinating agent in a reaction vehicle comprising a tertiary amide to afford a mixture; (ii) heating said mixture for a heating period in order to provide chlorination of sucrose-6-acylate at the 4,1,6 positions thereof; (iii) quenching the product stream of (ii) to produce a 4,1,6-trichloro-4,1,6-trideoxy-galactosucrose-6-acylate; wherein before quenching, a portion of said tertiary amide is removed by extraction into a solvent in which said tertiary amide is at least partially soluble. The tertiary amide is preferably N,N-dimethylformamide (DMF). The solvent used to extract the tertiary amide is preferably a hydrocarbon, particularly a cyclic or acyclic alkane comprising 5-7 carbon atoms, more particularly cyclohexane. The extraction is preferably performed at a temperature of 20-100°C and/or at a solvent to feed ratio of 1:1 to 8:1 w/w. The extracted tertiary amide may be removed from the extraction solvent by distillation; or via separation by addition of water to form a biphasic system, followed by separation of the two phases. The 4,1,6-trichloro-4,1,6-trideoxy-galactosucrose-6-acylate produced by be converted to sucralose. Embodiments relate to the preparation of 4,1,6-trichloro-4,1,6-trideoxy-galactosucrose-6-acetate (sucraluse-6-acetate).