Generation of phosphorus oxychloride as by-product from...

C - Chemistry – Metallurgy – 07 – H

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C07H 5/02 (2006.01) C07C 257/02 (2006.01) C07F 9/14 (2006.01)

Patent

CA 2606487

A process is described wherein after formation of first crop of Vilsmeier- Haack reagent by reacting Phosphorus Pentachloride with N,N-dimethylformamide to form a first crop of Vilsmeier reagent as insoluble crystals, a by-product of this reaction, the Phosphorus Oxy-Chloride, reacts with N,N- dimethylformamide to give a second crop of Vilsmeier reagent. This second crop of Vilsmeier reagent is soluble in DIV1F. This process makes it possible to double the yield of chlorinated substrate, such as sucrose-6-acetate or sucrose-6-benzoate, from the same quantity of Phosphorus Pentachloride.

Le procédé selon l'invention consiste à produire une première quantité de réactif de Vilsmeier-Haack par réaction de pentachlorure de phosphore avec du N,N-diméthylformamide de manière à former le réactif de Vilsmeier en tant que cristaux insolubles, puis à faire réagir un produit secondaire de cette réaction (oxychlorure de phosphore) avec du N,N-diméthylformamide de manière à former une deuxième quantité de réactif de Vilsmeier. Cette deuxième quantité de réactif de Vilsmeier est soluble dans DIV1F. Le procédé selon l'invention permet de doubler le rendement en substrat chloré tel que sucrose-6-acétate ou sucrose-6-benzoate à partir de la même quantité de pentachlorure de phosphore.

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