Hydrochloric Acid → Tosufloxacin hydrochloride

HRID 232486ノート

反応式

HRID 232486 の反応式
C([NH:4][CH:5]1[CH2:9][CH2:8][N:7]([C:10]2[C:27]([F:28])=[CH:26][C:13]([C:14]([C:16](=[CH:22]N(C)C)[C:17]([O:19]CC)=[O:18])=[O:15])=[C:12]([NH:29][C:30]3[CH:35]=[CH:34][C:33]([F:36])=[CH:32][C:31]=3[F:37])[N:11]=2)[CH2:6]1)(=O)C.[ClH:38]>C(O)C>[ClH:38].[NH2:4][CH:5]1[CH2:9][CH2:8][N:7]([C:10]2[N:11]=[C:12]3[C:13]([C:14](=[O:15])[C:16]([C:17]([OH:19])=[O:18])=[CH:22][N:29]3[C:30]3[CH:35]=[CH:34][C:33]([F:36])=[CH:32][C:31]=3[F:37])=[CH:26][C:27]=2[F:28])[CH2:6]1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 70391376ethyl 2-[6-(3-acetylamino-1-pyrrolidinyl)-2-(2,4-difluorophenylamino)-5-fluoronicotinoyl]-3-(N,N-dimethylamino)acrylate

生成物 1

HCID 10433396Tosufloxacin hydrochloride収率 85.4%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

In 4 ml of ethanol was suspended 200 mg of ethyl 2-[6-(3-acetylamino-1-pyrrolidinyl)-2-(2,4-difluorophenylamino)-5-fluoronicotinoyl]-3-(N,N-dimethylamino)acrylate, and 4 ml of 6N hydrochloric acid was added thereto, after which the resulting mixture was subjected to reaction under reflux for 3.5 hours. Subsequently, the solvent was removed by distillation under reduced pressure, and to the crystalline material thus obtained was added 2 ml of ethanol, after which crystals were collected by filtration to obtain 145 mg (yield 85.4%) of 7-(3-amino-1-pyrrolidinyl)-1-(2,4-difluorophenyl)-6-fluoro-1,4-dihydro-4-oxo-1,8-naphthyridine-3-carboxylic acid hydrochloride.

後処理

  1. additionwas added
  2. customafter which the resulting mixture was subjected to reaction
  3. temperatureunder reflux for 3.5 hours
  4. customSubsequently, the solvent was removed by distillation under reduced pressure
  5. customto the crystalline material thus obtained
  6. filtrationafter which crystals were collected by filtration

出典と根拠

ORDレコード
ord-4c74826effeb472a985ca42dfde685f8
出典データセット
uspto-grants-1989_07
特許番号
US04851535

反応ノート

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