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

HRID 986201

반응식

HRID 986201 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

반응 조건

온도
52 °C

실험 절차

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):

후처리

  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

출처 및 근거

ORD 기록
ord-8c945ae9b3824d6bae2b0672719f7246
출처 데이터셋
uspto-grants-1987_12
특허 번호
US04711880

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