Acetone → Ibandronate Sodium Anhydrous

HRID 229903

반응식

HRID 229903 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>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

5

반응물 3

HCID 180AcetoneHCID 14798Sodium HydroxideHCID 60852Ibandronate

생성물 1

HCID 23670359Ibandronate Sodium Anhydrous수율 100.5%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A solution of amorphous ibandronic acid (4.5 g) in water (11 ml) and sodium hydroxide (0.56 g, solid) was stirred at room temperature. The solution was added dropwise into acetone (100 ml). The resulting precipitate was stirred at room temperature for 16 hours. The precipitate was isolated by vacuum filtration, washed with acetone (2×10 ml), and dried in a vacuum oven at 50° C. for 24 hours to obtain 4.8 g of ibandronate sodium crystal form Q.

후처리

  1. customThe precipitate was isolated by vacuum filtration
  2. washwashed with acetone (2×10 ml)
  3. customdried in a vacuum oven at 50° C. for 24 hours

출처 및 근거

ORD 기록
ord-6a1b82f6e5fa454ca04159f11d79f476
출처 데이터셋
uspto-grants-2009_07
특허 번호
US07563918B2

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