Sodium Hydroxide → Alendronic Acid

HRID 871804

反応式

HRID 871804 の反応式
[CH2:1]([CH2:13][NH2:14])[CH2:2][C:3]([P:9]([O-:12])([OH:11])=[O:10])([P:5]([OH:8])([OH:7])=[O:6])[OH:4].O.O.O.[Na+].O.O.O.O.O.O.O.O.O.O.[O-:29][P:30]([O:33][P:34]([O-:37])([O-:36])=[O:35])(=[O:32])[O-:31].[Na+].[Na+].[Na+].[Na+].O.O.[Cl-].[Ca+2].[Cl-].C(CN)CC(P(O)(O)=O)(P(O)(O)=O)O.[O-]P(OP([O-])([O-])=O)(=O)[O-].[Cl-].[Ca+2].[Cl-].[OH-].[Na+]>O>[CH2:1]([CH2:13][NH2:14])[CH2:2][C:3]([P:5]([OH:7])([OH:8])=[O:6])([P:9]([OH:12])([OH:11])=[O:10])[OH:4].[O-:31][P:30]([O:33][P:34]([O-:37])([O-:36])=[O:35])(=[O:29])[O-:32]

参加物

9

反応物 6

HCID 14798Sodium HydroxideHCID 3084150Sodium pyrophosphate decahydrateHCID 5284359Calcium Chloride2 回HCID 6093260Calcium chloride, dihydrateHCID 23681107Alendronate SodiumHCID 131732545Alendronate pyrophosphate2 回

生成物 2

HCID 2088Alendronic AcidHCID 644102Pyrophosphate

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

0.81 g sodium alendronate trihydrate and 1.12 g sodium pyrophosphate decahydrate (Na4P2O7.10 H2O) were dissolved in 75 mL water. 1.21 g calcium chloride dihydrate was dissolved in 75 mL water. The temperature of the alendronate-pyrophosphate solution was brought to 40 to 50° C. Calcium chloride and sodium hydroxide solutions were simultaneously added to the alendronate-pyrophosphate solution while stirring to keep the pH at 7.4 until all the calcium chloride solution was added. The mixture was cooled to room temperature. The precipitate was collected by filtration and washed with water. The solid was dried in an oven at 105° C. overnight. 1.06 g of calcium complex salt of alendronate with pyrophosphate was thus obtained with a molecular ratio of 1:1.

後処理

  1. customwas brought to 40 to 50° C
  2. additionwas added
  3. filtrationThe precipitate was collected by filtration
  4. washwashed with water
  5. customThe solid was dried in an oven at 105° C. overnight

出典と根拠

ORDレコード
ord-3896abd22b354ab4b99336e731893355
出典データセット
uspto-grants-2015_03
特許番号
US08974801B2

関連ノート

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