Pamidronic Acid → Sodium (3-amino-1-hydroxy-1-phosphonopropyl)phosphonate

温度

52 °C

77.1 g of 3-amino-1-hydroxypropane-1,1-diphosphonic acid are suspended in 250 ml of demineralised water, and while stirring vigorously, 65.6 g of 40% aqueous sodium hydroxide solution are added. The rate of addition thereof is so regulated that the temperature of the reaction mixture during neutralisation rises to approximately 50° C. The reaction mixture is heated to 52° C. and inoculated and allowed to cool slowly to room temperature and left to stand overnight; the resulting salt cake is filtered with suction, washed with 120 ml of approximately 66% methanol and dried under 10-20 mbar at 150° C. until the weight is constant. Disodium 3-amino-1-hydroxypropane-1,1-diphosphonate is obtained in a substantially anhydrous crystalline form (modification A). This form is characterised by the following lattice spacings (d-values) and relative line intensities (intensities) of its X-ray powder pattern (camera according to Guinier-de-Wolff, radiation source: copper-Kα):

1. additionThe rate of addition
2. customrises to approximately 50° C
3. temperatureto cool slowly to room temperature
4. waitleft
5. filtrationthe resulting salt cake is filtered with suction
6. washwashed with 120 ml of approximately 66% methanol
7. customdried under 10-20 mbar at 150° C. until the weight

ORDレコード

ord-8c945ae9b3824d6bae2b0672719f7246

出典データセット

uspto-grants-1987_12

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04711880