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

HRID 980777

반응식

HRID 980777 반응식
[NH2:1][CH2:2][CH2:3][C:4]([OH:13])([P:9]([OH:12])(=[O:11])[OH:10])[P:5]([OH:8])(=[O:7])[OH:6].[OH-].[Na+:15]>O>[NH2:1][CH2:2][CH2:3][C:4]([OH:13])([P:5]([OH:8])(=[O:6])[OH:7])[P:9]([O-:12])(=[O:10])[O-:11].[Na+:15].[Na+:15]

참가 물질

4

반응물 2

HCID 4674Pamidronic AcidHCID 14798Sodium Hydroxide

생성물 1

HCID 44181920Sodium (3-amino-1-hydroxy-1-phosphonopropyl)phosphonate

시약·촉매·용매 1

HCID 962Water용매

실험 절차

50.0 g of 3-amino-1-hydroxypropane-1,1-diphosphonic acid are suspended in 370 ml of demineralised water and, while stirring, heated to 50°. 56.6 g of 30% aqueous sodium hydroxide solution are then added in such a manner that the temperature of the reaction mixture during neutralisation rises to 59°. The reaction mixture is heated to 65°, filtered hot over diatomaceous earth, heated to 75° and, while stirring, 300 ml of water are distilled off under reduced pressure. The mixture is allowed to cool to approximately 52°, and inoculated and allowed to cool slowly to room temperature while stirring, crystallisation starting at approximately 45°. The crystals are left to stand in the mother liquor overnight, stirred for 1 hour in an ice bath to complete the reaction, filtered with suction, washed with a little ice-water and dried under reduced pressure at room temperature until the weight is constant. Disodium 3-amino-1-hydroxypropane-1,1-diphosphonate is obtained in the granular-crystalline crystal form of modification B which contains less water than the crystal modification containing water of crystallisation according to the invention (modification E). 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):

후처리

  1. temperatureheated to 50°
  2. customrises to 59°
  3. temperatureThe reaction mixture is heated to 65°
  4. filtrationfiltered hot over diatomaceous earth
  5. temperatureheated to 75°
  6. stirringwhile stirring
  7. distillation300 ml of water are distilled off under reduced pressure
  8. temperatureto cool to approximately 52°
  9. stirringwhile stirring
  10. customcrystallisation
  11. customstarting at approximately 45°
  12. waitThe crystals are left
  13. customto stand in the mother liquor overnight
  14. stirringstirred for 1 hour in an ice bath
  15. customthe reaction
  16. filtrationfiltered with suction
  17. washwashed with a little ice-water
  18. customdried under reduced pressure at room temperature until the weight

출처 및 근거

ORD 기록
ord-a3eddf99687645d0ad010897b64dcd89
출처 데이터셋
uspto-grants-1987_01
특허 번호
US04639338

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