Acetone → Ibandronate Sodium Anhydrous

HRID 229903

反応式

HRID 229903 の反応式
[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][N:6]([CH2:8][CH2:9][C:10]([P:16]([OH:19])([OH:18])=[O:17])([P:12]([OH:15])([OH:14])=[O:13])[OH:11])[CH3:7].[OH-].[Na+:21].CC(C)=O>O>[CH3:1][CH2:2][CH2:3][CH2:4][CH2:5][N:6]([CH2:8][CH2:9][C:10]([P:16]([O-:19])([OH:18])=[O:17])([P:12]([OH:15])([OH:14])=[O:13])[OH:11])[CH3:7].[Na+:21]

参加物

5

反応物 3

HCID 180AcetoneHCID 14798Sodium HydroxideHCID 60852Ibandronate

生成物 1

HCID 23670359Ibandronate Sodium Anhydrous収率 100.5%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A solution of amorphous ibandronic acid (4.5 g) in water (11 ml) and sodium hydroxide (0.56 g, solid) was stirred at room temperature. The solution was added dropwise into acetone (100 ml). The resulting precipitate was stirred at room temperature for 16 hours. The precipitate was isolated by vacuum filtration, washed with acetone (2×10 ml), and dried in a vacuum oven at 50° C. for 24 hours to obtain 4.8 g of ibandronate sodium crystal form Q.

後処理

  1. customThe precipitate was isolated by vacuum filtration
  2. washwashed with acetone (2×10 ml)
  3. customdried in a vacuum oven at 50° C. for 24 hours

出典と根拠

ORDレコード
ord-6a1b82f6e5fa454ca04159f11d79f476
出典データセット
uspto-grants-2009_07
特許番号
US07563918B2

関連ノート

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