Distillative purification of 2,5-dioxo-1-oxa-2-phospholanes

B - Operations – Transporting – 01 – D

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B01D 3/10 (2006.01) C07F 9/6571 (2006.01)

Patent

CA 1055877

ABSTRACT OF THE DISCLOSURE: 2,5 dioxo-1-oxa-2-phospholanes of the general formula: Image in which R1 stands for a n alkyl radical having form 1 to 4 carbon atoms, or a phenyl radical, and R2 and R3 each stand for hydrogen or CH3, are distillativelypuri- fied. To this end the respective crude compound is pre- heated to 120 to 160°C and fed to the head of a distilling column provided with a plurality of individually heat- able trays maintained at temperatures increasing from the upper-most tray to the lowermost, the uppermost tray in the column being maintained at 160 to 200°C, the pressure at the head of the column being 20 to 200 mm Hg, preferably 50 to 120 mm Hg; an inert gas preheated at 160 to 200°C is introduced countercurrently at the base of the column; those impurities having a boiling point lower than that of the respective 2,5-dioxo-1-oxa- 2-phospholane are withdrawn overhead together with the inert gas; the 2,5-dioxo-1-oxa-2-phospholane thus freed from low-boiling impurities is withdrawn from the base of the distilling column and passed to a film evapora- tor; and the 2,5-dioxo-1-oxa-2-phospholane is distilled off from higher-boiling impurities in the film evapora- tor under a pressure of 0.1 to 5 mm Hg.

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