Sodium Hydroxide → Ibandronate Sodium Anhydrous

HRID 229899

반응식

HRID 229899 반응식
[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]

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 60852Ibandronate

생성물 1

HCID 23670359Ibandronate Sodium Anhydrous수율 102.9%

시약·촉매·용매 1

HCID 3776Isopropanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-91f007a0f36847afaceb9e22d0da541f
출처 데이터셋
uspto-grants-2009_07
특허 번호
US07563918B2

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