Sodium Hydroxide → Ibandronate Sodium Anhydrous

HRID 229899

反応式

HRID 229899 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(O)C>[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 102.9%

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

A slurry of amorphous ibandronic acid (5 g) in IPA (50 ml) was heated to reflux temperature. Sodium hydroxide (0.63 g, solid) was added, and the reaction mixture was heated at reflux temperature for an additional 4 hours to obtain a pH of 4.19. Then the reaction mixture was cooled to room temperature. Further cooling was performed using an ice-bath. The precipitate was filtered, washed with IPA (2×25 ml), and dried in a vacuum oven at 50° C. for 24 hours to give 5.5 g of ibandronate sodium crystal form K. Form K can exhibit a weight loss of about 10% to about 14% in TGA.

後処理

  1. temperatureto reflux temperature
  2. temperaturethe reaction mixture was heated
  3. temperatureat reflux temperature for an additional 4 hours
  4. customto obtain a pH of 4.19
  5. temperatureFurther cooling
  6. filtrationThe precipitate was filtered
  7. washwashed with IPA (2×25 ml)
  8. customdried in a vacuum oven at 50° C. for 24 hours

出典と根拠

ORDレコード
ord-91f007a0f36847afaceb9e22d0da541f
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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