Sodium Hydroxide → Ibandronate Sodium Anhydrous

HRID 229901

反応式

HRID 229901 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>[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

4

反応物 2

HCID 14798Sodium HydroxideHCID 60852Ibandronate

生成物 1

HCID 23670359Ibandronate Sodium Anhydrous収率 91.5%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

A slurry of amorphous ibandronic acid (4.6 g) in acetone (96 ml) was heated to reflux temperature. Sodium hydroxide (0.58 g, solid) was added, and the reaction mixture was stirred at reflux temperature for an additional 10 hours to obtain a pH of 3.35. Then the reaction mixture was cooled to room temperature. Further cooling was performed using an ice-bath. The white solid was filtered, washed with acetone (2×25 ml), and dried in a vacuum oven at 50° C. for 21 hours to give 4.5 g of ibandronate sodium crystal form Q.

後処理

  1. temperatureto reflux temperature
  2. temperatureat reflux temperature for an additional 10 hours
  3. customto obtain a pH of 3.35
  4. temperatureFurther cooling
  5. filtrationThe white solid was filtered
  6. washwashed with acetone (2×25 ml)
  7. customdried in a vacuum oven at 50° C. for 21 hours

出典と根拠

ORDレコード
ord-96bce559a94448e1b859bceddf2c41fe
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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