Sodium Hydroxide → Alendronate sodium anhydrous

HRID 651846

반응식

HRID 651846 반응식
[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]

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 15585620Alendronic acid monohydrate2회

생성물 1

HCID 16760285Alendronate sodium anhydrous

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

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.

후처리

  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.)

출처 및 근거

ORD 기록
ord-48e7466709854a0ebc8d253c998569b8
출처 데이터셋
uspto-grants-2001_08
특허 번호
US06281381B1

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