Levofloxacin → Levofloxacin Hydrate

HRID 31371

반응식

HRID 31371 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>CCCCO>[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].[OH2:4]

참가 물질

3

반응물 1

HCID 149096Levofloxacin

생성물 1

HCID 3033924Levofloxacin Hydrate수율 118.5%

시약·촉매·용매 1

HCID 2631-Butanol용매

실험 절차

1 g of levofloxacin crude was put in suspension in 7 ml of n-BuOH. The mixture was heated to reflux temperature until complete dissolution of the material. Then the solution was cooled to RT over a period of 2.5 hours. The precipitate was filtrated under vacuum, washed with n-BuOH and dried at 60° C. in a vacuum oven to give 810 mg (81%) of purified levofloxacin hemihydrate.

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 n-BuOH
  6. customdried at 60° C. in a vacuum oven

출처 및 근거

ORD 기록
ord-edc8959a3ec14e8e9a416f73ba49e7be
출처 데이터셋
uspto-grants-2008_09
특허 번호
US07425628B2

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