Continuous preparation of phosphoric acid alkyl ester dichloride

Chemistry of carbon compounds – Dipeptides – e.g. – aspartame – anserine – carnosine – etc.

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C07F 914

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active

042960479

ABSTRACT:
In the preparation of a phosphoric acid alkyl ester dichloride by reacting phosphorus oxychloride with an aliphatic alcohol according to the equation ##STR1## in which R represents C.sub.1 -C.sub.5 -alkyl,
the improvement which comprises carrying out the reaction continuously at a temperature of about 10.degree. to 50.degree. C. using an excess of phosphorus oxychloride of about 5 to 40%. The excess phosphorus oxychloride is reacted with the alcohol by continuous mixing, the reaction mixture is cooled, substantially all the hydrogen chloride formed is then separated off in a preliminary degassing stage, the reaction mixture is worked up in a distillation column, the unreacted phosphorus oxychloride and any diluent is separated off over the top and condensed, the condensate is recycled to the reaction and the corresponding alkyl ester dichloride is removed continuously as the bottom product.

REFERENCES:
patent: 1945183 (1934-01-01), Clemmensen
patent: 2487859 (1949-11-01), Dickey et al.
patent: 2750399 (1956-06-01), Gamrath et al.
patent: 2960527 (1960-11-01), Granze et al.
Houben-Weyl, vol. 2, p. 212.

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