Sodium Hydroxide → Alendronate sodium anhydrous

HRID 651843

반응식

HRID 651843 반응식
[OH-].[Na+:2].[CH2:3]([CH2:15][NH2:16])[CH2:4][C:5]([P:11]([OH:14])([OH:13])=[O:12])([P:7]([OH:10])([OH:9])=[O:8])[OH:6].O>C(O)C.O>[CH2:3]([CH2:15][NH2:16])[CH2:4][C:5]([P:7]([O-:9])([OH:10])=[O:8])([P:11]([OH:14])([OH:13])=[O:12])[OH:6].[Na+:2]

참가 물질

5

반응물 2

HCID 14798Sodium HydroxideHCID 15585620Alendronic acid monohydrate

생성물 1

HCID 16760285Alendronate sodium anhydrous수율 96%

시약·촉매·용매 2

HCID 702Ethanol용매2회HCID 962Water용매

실험 절차

A 250 ml flask was fitted with a mechanical stirrer, a thermometer, and a reflux condenser. The flask was charged with 38.2 ml of a solution of sodium hydroxide in ethanol (0.49N, 18.7 mmol), 4.8 ml of ethanol, water (0 to 100 mol. eq., according to the crystal form desired), and 5 g (18.7 mmol) of alendronic acid monohydrate. The reaction mixture was boiled with vigorous stirring for about 15 hours until stability of pH of the liquid phase was reached (approx. pH 7). After cooling of the reaction mixture to ambient temperature the precipitate was filtered, washed with absolute ethanol, and dried overnight in a vacuum oven (10-15 mm Hg, ambient temperature) to give 96-99% sodium alendronate having the following crystalline forms: crystalline Form B, when 0-4 (preferably 0-2) mol. eq. water were used; crystalline Form F, when 3-5 mol. eq. water were used; crystalline Form E, when 11-13 (preferably 12) mol. eq. water were used; and crystalline Form G, when 15-100 (preferably 20-80) mol. eq. water were used.

후처리

  1. customA 250 ml flask was fitted with a mechanical stirrer
  2. filtrationwas filtered
  3. washwashed with absolute ethanol
  4. customdried overnight in a vacuum oven (10-15 mm Hg, ambient temperature)

출처 및 근거

ORD 기록
ord-9af70c6f8dec4746a2de9c57171d110f
출처 데이터셋
uspto-grants-2001_08
특허 번호
US06281381B1

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