Levofloxacin → Levofloxacin Hydrate

HRID 31376

反応式

HRID 31376 の反応式
[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]

参加物

3

反応物 1

HCID 149096Levofloxacin

生成物 1

HCID 3033924Levofloxacin Hydrate収率 84%

試薬・触媒・溶媒 1

HCID 6569Methyl Ethyl Ketone溶媒

反応条件

温度
-5 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-5ef30b4014b14c6b9ef8a9cf7daa197a
出典データセット
uspto-grants-2008_09
特許番号
US07425628B2

関連ノート

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