Sodium Hydroxide → Alendronate sodium anhydrous

HRID 651846

反応式

HRID 651846 の反応式
[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]

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 15585620Alendronic acid monohydrate2 回

生成物 1

HCID 16760285Alendronate sodium anhydrous

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

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, and dried overnight in a vacuum oven (10-15 mm Hg, 40-50° C.) to give 26.2 g of alendronate sodium, having crystalline Form G.

後処理

  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. customdried overnight in a vacuum oven (10-15 mm Hg, 40-50° C.)

出典と根拠

ORDレコード
ord-48e7466709854a0ebc8d253c998569b8
出典データセット
uspto-grants-2001_08
特許番号
US06281381B1

関連ノート

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