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

HRID 986203

反応式

HRID 986203 の反応式
[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]

参加物

4

反応物 2

HCID 4674Pamidronic AcidHCID 14798Sodium Hydroxide

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-e3bc51619ff1425b98e5412573fba3c9
出典データセット
uspto-grants-1987_12
特許番号
US04711880

関連ノート

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