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

HRID 980775

반응식

HRID 980775 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

32.7 g of 3-amino-1-hydroxypropane-1,1-diphosphonic acid are suspended in 106 ml of demineralised water. The suspension is heated to 35° and, while stirring vigorously, 28 ml of 30% aqueous sodium hydroxide solution are added dropwise at such a rate that the temperature of the reaction mixture rises to 54°. A clear solution is obtained initially from which crystallisation begins immediately. The whole is allowed to cool slowly to room temperature while stirring is continued, and then stirred for 8 hours at room temperature, filtered with suction, washed with a mixture of 2 parts by volume of methanol and 1 part by volume of water and dried at 30° under approximately 20 mbar until the weight is constant. Disodium 3-amino-1-hydroxypropane-1,1-diphosphonate is obtained in the novel crystal form containing water of crystallisation (modification E), the IR spectrum of which is identical to that of the product obtained according to Example 1.

후처리

  1. temperatureThe suspension is heated to 35°
  2. customrises to 54°
  3. customA clear solution is obtained initially from which crystallisation
  4. stirringwhile stirring
  5. stirringstirred for 8 hours at room temperature
  6. filtrationfiltered with suction
  7. washwashed with a mixture of 2 parts by volume of methanol and 1 part by volume of water
  8. customdried at 30° under approximately 20 mbar until the weight

출처 및 근거

ORD 기록
ord-ffd6b641524e42ce91eb67f5cb092202
출처 데이터셋
uspto-grants-1987_01
특허 번호
US04639338

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