Sodium Hydroxide → Alendronic Acid

HRID 871804

반응식

HRID 871804 반응식
[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]

참가 물질

9

반응물 6

HCID 14798Sodium HydroxideHCID 3084150Sodium pyrophosphate decahydrateHCID 5284359Calcium Chloride2회HCID 6093260Calcium chloride, dihydrateHCID 23681107Alendronate SodiumHCID 131732545Alendronate pyrophosphate2회

생성물 2

HCID 2088Alendronic AcidHCID 644102Pyrophosphate

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-3896abd22b354ab4b99336e731893355
출처 데이터셋
uspto-grants-2015_03
특허 번호
US08974801B2

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