Levofloxacin → Levofloxacin Hydrate

HRID 31376

반응식

HRID 31376 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>CCC(C)=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].[OH2:4]

참가 물질

3

반응물 1

HCID 149096Levofloxacin

생성물 1

HCID 3033924Levofloxacin Hydrate수율 84%

시약·촉매·용매 1

HCID 6569Methyl Ethyl Ketone용매

반응 조건

온도
-5 °C

실험 절차

1.5 g of levofloxacin crude was put in suspension in 15 ml of MEK. The mixture was heated to reflux temperature until complete dissolution of the material. Then the solution was cooled to −5° C. over a period of 3 hours. The precipitate was filtrated under vacuum, washed with 1.5 ml of MEK and dried at 30° C. in a vacuum oven to give 840 mg (84%) 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 1.5 ml of MEK
  6. customdried at 30° C. in a vacuum oven

출처 및 근거

ORD 기록
ord-5ef30b4014b14c6b9ef8a9cf7daa197a
출처 데이터셋
uspto-grants-2008_09
특허 번호
US07425628B2

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