Tate & Lyle Technology Limited

Thomas Eilers

David Dentel

Halil Aktas

Edward Micinski

The present invention relates to a method for the chlorination of a sucrose-6-acylate to produce a 4,1',6&#x2032;-trichloro-4,1&#x2032;,6&#x2032;-trideoxy-galactosucrose-6-acylate wherein said method includes steps of:

Liquid-liquid extraction of DMF

A method of obtaining purified DMF from a mixture comprising DMF and hydrogen chloride (HCl) involving distillation is provided.

DMF distillation

There is provided a method for the chlorination of a sucrose-6-acylate to produce a 4,1',6&#x2032;-trichloro-4,1&#x2032;,6&#x2032;-trideoxy-galactosucrose-6-acylate, wherein said method comprises the following steps (i) to (v): (i) providing a first component comprising sucrose-6-acylate; (ii) providing a second component comprising a chlorinating agent; (iii) combining said first component and said second component to afford a mixture; (iv) heating said mixture for a heating period in order to provide chlorination of sucrose-6-acylate at the 4, 1&#x2032; and 6&#x2032; positions thereof; (v) quenching said mixture to produce a 4,1&#x2032;,6&#x2032;-trichloro-4,1&#x2032;,6&#x2032;-trideoxy-galactosucrose-6-acylate; wherein at least one of said first component and said second component comprises a reaction vehicle, and said reaction vehicle comprises a tertiary amide; and wherein said mixture comprises a cosolvent during a least a portion of the heating period of step (iv), wherein said cosolvent comprises perfluorooctane.

Chlorination of sucrose-6-esters

There is provided a method for the chlorination of a sucrose-6-acylate to produce a 4,1',6&#x2032;-trichloro-4,1&#x2032;,6&#x2032;-trideoxy-galactosucrose-6-acylate, wherein said method comprises the following steps (i) to (v): (i) providing a first component comprising sucrose-6-acylate; (ii) providing a second component comprising a chlorinating agent; (iii) combining said first component and said second component to afford a mixture; (iv) heating said mixture for a heating period in order to provide chlorination of sucrose-6-acylate at the 4, 1&#x2032; and 6&#x2032; positions thereof; (v) quenching said mixture to produce a 4,1&#x2032;,6&#x2032;-trichloro-4,1&#x2032;,6&#x2032;-trideoxy-galactosucrose-6-acylate; wherein at least one of said first component and said second component comprises a reaction vehicle, and said reaction vehicle comprises a tertiary amide; and wherein said mixture comprises a cosolvent during a least a portion of the heating period of step (iv), wherein said cosolvent comprises dimethylacetamide (DMAc).

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Arlington Heights, IL, United States of America

Thomas Eilers