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

HRID 986202

반응식

HRID 986202 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 Acid2회HCID 14798Sodium Hydroxide2회

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

실험 절차

70.0 kg of 3-amino-1-hydroxypropane-1,1-diphosphonic acid are suspended while stirring in 140 liters of demineralised water. The suspension is heated to 65°-70° and 59.9 liters, (79.5 kg) of 30% aqueous sodium hydroxide solution are added at such a rate that the temperature of the reaction mixture rises to approximately 85° with the formation of a clear solution. The pH value of the solution should be between 7.2 and 7.5. It can be finely adjusted if necessary by the addition of small amounts of 30% sodium hydroxide solution or of 3-amino-1-hydroxypropane-1,1-diphosphonic acid. The solution is cleared by filtering through a filter that is coated with a small quantity of diatomaceous earth and has been preheated to 75°-80° into a vessel preheated to the same temperature. The solution is inoculated, and, while stirring, cooled in the course of 2 hours to 20°-25°, 70 liters of 96% ethanol are added in the course of a further 2 hours while stirring, the mixture is then cooled to 0°-5° in the course of 1 hour and the reaction is completed by stirring at this temperature for at least 1 hour. The mother liquor is then centrifuged off and the residue is washed in portions with a mixture of 25 litres of ethanol and 45 litres of demineralised water. The whole is centrifuged thoroughly and dried in a vacuum cabinet at 35°-40° until the weight is constant (approximately 24 hours). 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 65°-70°
  2. customrises to approximately 85° with the formation of a clear solution
  3. filtrationby filtering through
  4. filtrationa filter that
  5. customhas been preheated to 75°-80° into a vessel
  6. temperaturecooled in the course of 2 hours to 20°-25°
  7. addition70 liters of 96% ethanol are added in the course of a further 2 hours
  8. stirringwhile stirring
  9. temperaturethe mixture is then cooled to 0°-5° in the course of 1 hour
  10. stirringby stirring at this temperature for at least 1 hour
  11. washthe residue is washed in portions with a mixture of 25 litres of ethanol and 45 litres of demineralised water
  12. customdried in a vacuum cabinet at 35°-40° until the weight
  13. custom(approximately 24 hours)

출처 및 근거

ORD 기록
ord-05ab016ee0824dbbb9c8944754a8df16
출처 데이터셋
uspto-grants-1987_12
특허 번호
US04711880

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