Sodium Hydroxide → Alendronate sodium anhydrous

HRID 651843ノート

反応式

HRID 651843 の反応式
[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]

参加物

5

反応物 2

HCID 14798Sodium HydroxideHCID 15585620Alendronic acid monohydrate

生成物 1

HCID 16760285Alendronate sodium anhydrous収率 96%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒2 回HCID 962Water溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-9af70c6f8dec4746a2de9c57171d110f
出典データセット
uspto-grants-2001_08
特許番号
US06281381B1

反応ノート

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