Sodium Hydroxide → Ibandronate Sodium Anhydrous

HRID 229898

反応式

HRID 229898 の反応式
[OH-].[Na+:2].[CH3:3][CH2:4][CH2:5][CH2:6][CH2:7][N:8]([CH2:10][CH2:11][C:12]([P:18]([OH:21])([OH:20])=[O:19])([P:14]([OH:17])([OH:16])=[O:15])[OH:13])[CH3:9]>O.CC(O)C>[CH3:3][CH2:4][CH2:5][CH2:6][CH2:7][N:8]([CH2:10][CH2:11][C:12]([P:18]([O-:21])([OH:20])=[O:19])([P:14]([OH:17])([OH:16])=[O:15])[OH:13])[CH3:9].[Na+:2]

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 60852Ibandronate

生成物 1

HCID 23670359Ibandronate Sodium Anhydrous収率 97.3%

試薬・触媒・溶媒 1

HCID 21889133Propan-2-ol--water (1/1)溶媒2 回

実験手順

A solution of sodium hydroxide (0.63 g) in water:IPA (60:40 v/v, 19 ml) was added dropwise to a solution of amorphous ibandronic acid (5 g) in water:IPA (60:40 v/v, 106 ml) at reflux temperature. The reaction mixture was heated at reflux temperature for an additional 30 minutes to obtain a pH of 4.14. Then the reaction mixture was cooled to room temperature and stirred for 16 hours. 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 23 hours to give 5.2 g of ibandronate sodium crystal form F.

後処理

  1. temperatureat reflux temperature
  2. temperatureThe reaction mixture was heated
  3. temperatureat reflux temperature for an additional 30 minutes
  4. customto obtain a pH of 4.14
  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 23 hours

出典と根拠

ORDレコード
ord-194c5ced0b074941b25f4ba2433311e8
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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