Method for purifying aminomethylenephosphonic acids for pharmace

Details Method for purifying aminomethylenephosphonic acids for pharmace Method for purifying aminomethylenephosphonic acids for pharmace

1989-08-04

1990-06-26

Springer, David B.

Organic compounds -- part of the class 532-570 series

Organic compounds

Unsubstituted hydrocarbyl chain between the ring and the -c-...

562 14, 562 16, C07F 938, C07F 966

Patent

active

049373331

ABSTRACT:
High purity ethylenediaminetetra(methylenephosphonic acid) and 1,4,7,10-tetraazacyclododecane-1,4,7,10-tetra(methylenephosphonic acid) are prepared by dissolving the aminomethylenephosphonic acid in an aqueous base, acidifying with a mineral acid at an elevated temperature to precipitate the crystals, maintaining the solution at an elevated temperature for a period of time sufficient to assure crystallization, cooling to a lower temperature and maintaining at that temperature for a time sufficient to precipitate the crystals and filtering the resulting crystals at that temperature, washing the crystals with water and recovering the desired high purity aminophosphonic acid. The ethylenediaminetetra(methylenephosphonic acid) is obtained in a purer state during its synthesis if the crystals are filtered hot without prior cooling.

REFERENCES:
patent: 2599807 (1952-06-01), Bersworth
patent: 3288846 (1966-11-01), Irani et al.
patent: 3738937 (1973-06-01), Kautsky
Ixv. Akad. Nauk SSSR, Ser. Khim, 835, 1984.
Izv. Akad. Nauk SSSR, Ser. Khim, 844, 1984.
J. Magn. Reson. 76, 528 (1988).

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