Sodium Hydroxide → Alendronate sodium anhydrous

HRID 651844

Reaktionsgleichung

Reaktionsgleichung von HRID 651844
[CH2:1]([CH2:13][NH2:14])[CH2:2][C:3]([P:9]([OH:12])([OH:11])=[O:10])([P:5]([OH:8])([OH:7])=[O:6])[OH:4].O.[OH-].[Na+:17]>C(O)C>[CH2:1]([CH2:13][NH2:14])[CH2:2][C:3]([P:5]([O-:7])([OH:8])=[O:6])([P:9]([OH:12])([OH:11])=[O:10])[OH:4].[Na+:17]

Komponenten

4

Edukt 2

HCID 14798Sodium HydroxideHCID 15585620Alendronic acid monohydrate2×

Produkt 1

HCID 16760285Alendronate sodium anhydrous

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel2×

Versuchsvorschrift

A one liter flask was fitted with a mechanical stirrer, a thermometer, and a reflux condenser. The flask was charged with alendronic acid monohydrate (25 g, 0.094 mol) and aqueous ethanol. The mixture was heated to boiling with stirring. The aqueous ethanolic sodium hydroxide was added dropwise to the suspension of alendronic acid monohydrate in aqueous ethanol for 3 hours at reflux with vigorously stirring. Then the mixture was stirred at reflux for additional 15 hours. The mixture was cooled to room temperature with stirring. The solid was filtered, washed with absolute ethanol, then with absolute ethyl ether, and dried overnight in a vacuum oven (10-15 mm Hg, ambient temperature) to give 26.2 g of alendronate sodium, having crystalline Form G.

Aufarbeitung

  1. customA one liter flask was fitted with a mechanical stirrer
  2. temperatureThe mixture was heated
  3. temperatureat reflux
  4. stirringwith vigorously stirring
  5. stirringThen the mixture was stirred
  6. temperatureat reflux for additional 15 hours
  7. stirringwith stirring
  8. filtrationThe solid was filtered
  9. washwashed with absolute ethanol
  10. dry with materialwith absolute ethyl ether, and dried overnight in a vacuum oven (10-15 mm Hg, ambient temperature)

Quellen und Nachweise

ORD-Eintrag
ord-77bae6d4e7584513b202027ad9749d29
Quelldatensatz
uspto-grants-2001_08
Patentnummer
US06281381B1

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