Risedronate → Sodium hydrogen [1-hydroxy-1-phosphono-2-(pyridin-3-yl)ethyl]phosphonate

Temperatur

50 °C

A solution of sodium hydroxide (7.4 g, 1 eq.) in a mixture of water/ethanol (50%, v/v) (150 ml) was added drop-wise to a suspension of risedronic acid (50 g) and 5 g of EDTA (ca. 10% on a dry per-weight basis) in a mixture of water/ethanol (50%, v/v) (850 ml) at reflux temperature. The reaction mixture was stirred at reflux temperature until the pH was stable at about 4.2-4.7. The reaction mixture was cooled to a temperature of about 50° C. The precipitate was then filtered, washed twice with 50 ml mixture of water/ethanol (50%, v/v) and then with ethanol (1×50 ml) and dried over night at 50° C. to give 48.5 g (85%) of sodium risedronate white crystal substance of form B (water content by thermogravimetric analysis was 5.5%-7.5%). Less than 50 ppm of iron was found in the product by AES.

1. additionwas added drop-wise
2. customa dry per-weight basis)
3. additionin a mixture of water/ethanol (50%, v/v) (850 ml)
4. temperatureat reflux temperature
5. temperatureat reflux temperature until the pH
6. filtrationThe precipitate was then filtered
7. washwashed twice with 50 ml mixture of water/ethanol (50%, v/v)
8. dry with materialwith ethanol (1×50 ml) and dried over night at 50° C.

ORD-Eintrag

ord-cc8a6f9604c84ef9bb8b8526205a5763

Quelldatensatz

uspto-grants-2008_04

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07358360B2