Sodium Hydroxide → Ibandronate Sodium Anhydrous

HRID 229901

반응식

HRID 229901 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(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]

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 60852Ibandronate

생성물 1

HCID 23670359Ibandronate Sodium Anhydrous수율 91.5%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-96bce559a94448e1b859bceddf2c41fe
출처 데이터셋
uspto-grants-2009_07
특허 번호
US07563918B2

연결된 노트

불러오는 중…