Levofloxacin → Levofloxacin Hydrate

HRID 31373

반응식

HRID 31373 반응식
[CH3:1][C@@H:2]1[N:23]2[C:6]3[C:7]([C:19]([C:21]([C:24]([OH:26])=[O:25])=[CH:22]2)=[O:20])=[CH:8][C:9]([F:18])=[C:10]([N:11]2[CH2:16][CH2:15][N:14]([CH3:17])[CH2:13][CH2:12]2)[C:5]=3[O:4][CH2:3]1.S(S([O-])=O)([O-])(=O)=[O:28].[Na+].[Na+]>CCCCO.O>[CH3:1][C@@H:2]1[N:23]2[CH:22]=[C:21]([C:24]([OH:26])=[O:25])[C:19]([C:7]3=[CH:8][C:9]([F:18])=[C:10]([N:11]4[CH2:16][CH2:15][N:14]([CH3:17])[CH2:13][CH2:12]4)[C:5](=[C:6]23)[O:4][CH2:3]1)=[O:20].[CH3:1][C@@H:2]1[N:23]2[CH:22]=[C:21]([C:24]([OH:26])=[O:25])[C:19]([C:7]3=[CH:8][C:9]([F:18])=[C:10]([N:11]4[CH2:16][CH2:15][N:14]([CH3:17])[CH2:13][CH2:12]4)[C:5](=[C:6]23)[O:4][CH2:3]1)=[O:20].[OH2:28]

참가 물질

4

반응물 2

HCID 149096LevofloxacinHCID 656671Sodium Pyrosulfite

생성물 1

HCID 3033924Levofloxacin Hydrate수율 3,079.7%

시약·촉매·용매 1

HCID 22253497Water butanol용매

실험 절차

1.5 g of levofloxacin crude and 10 mg of sodium metabisulfite were put in suspension in 6 ml of a mixture n-BuOH:H2O (9:1) under nitrogen atmosphere. The mixture was heated to reflux temperature until complete dissolution of the material. Then the solution was cooled to RT over a period of 1.5 hours. The precipitate was filtrated under vacuum, washed with a mixture n-BuOH:H2O (9:1) (4 ml) and dried at 60° C. in a vacuum oven to give 1.2 g (81%) of purified levofloxacin hemihydrate. The purified levofloxacin hemihydrate contained virtually no N-oxide levofloxacin.

후처리

  1. temperatureThe mixture was heated
  2. temperatureto reflux temperature
  3. dissolutionuntil complete dissolution of the material
  4. filtrationThe precipitate was filtrated under vacuum
  5. washwashed with a mixture n-BuOH:H2O (9:1) (4 ml)
  6. customdried at 60° C. in a vacuum oven

출처 및 근거

ORD 기록
ord-ddc7ca042d31442d9c83c909303e04dd
출처 데이터셋
uspto-grants-2008_09
특허 번호
US07425628B2

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