32573-98-1Relevant articles and documents
Optimized synthesis of etidronate
Kovacs, Rita,Nagy, David Illes,Gruen, Alajos,Balogh, Gyoergy Tibor,Garadnay, Sandor,Greiner, Istvan,Keglevich, Gyoergy
, p. 733 - 737 (2013)
The synthesis of Etidronate (as the disodium salt) by the reaction of acetic acid with phosphorus trichloride/phosphorus acid in methanesulfonic acid was studied and optimized. We showed that it is enough to use 3.2 equivalents of the phosphorus trichlori
Investigation of Physical Properties of Disodium Etidronate Tetrahydrate and Application of Phosphorus K-Edge X-Ray Absorption Near-Edge Structure Spectroscopy
Ito, Naoya,Hashizuka, Takahiko,Ito, Masataka,Suzuki, Hironori,Noguchi, Shuji
, p. 2147 - 2155 (2021/12/22)
Purpose: Disodium etidronate is a bisphosphonate, compounds that are widely used in the treatment of bone disorders such as osteoporosis and Paget’s disease. We investigated the physical properties of disodium etidronate tetrahydrate crystal, form I. Methods: We used X-ray powder diffraction (XRPD), thermal analysis, dynamic vapor sorption (DVS), X-ray single crystal structure analysis, and phosphorus K-edge X-ray absorption near-edge structure (XANES) spectroscopy for the first time. Results: XRPD and thermal analyses demonstrated that form I was dehydrated and transformed to an amorphous form, to a crystalline form II, and finally to a form III by heating. DVS measurements revealed that the amorphous form, form II, and form III were rehydrated to form I by humidification, and form I was stable even at 0% relative humidity. These results indicate that form I is the most stable solid-state under ambient conditions and is suitable as an API for manufacture in solid formulations. The phosphorus K-edge XANES spectra differed among form I, the amorphous form, and form II, which may be ascribed to the difference in the coordinate bond schemes between the phosphate moieties and sodium ions. The results demonstrated that the phosphorus K-edge XANES spectroscopy could be applied to the identification or the discrimination of crystal forms of the APIs containing phosphate moieties. Conclusions: Acquired information about physical properties are crucial for manufacturing of solid formulations of disodium etidronate. XANES spectroscopy is a promising alternative method for evaluating the solid-state forms of APIs.
Aminohydroxypropane esters of hydroxyethylidenebisphosphoric acid.
Chuiko, Alexey,Philonenko, Ludmila,Borisevich, Anatoly,Lozinsky, Miron
, p. 66 (2007/10/03)
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