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Trifluoroacetic acid → Despropylene Gatifloxacin

HRID 1270078
ノート
印刷プレビュー

反応式

HRID 1270078 の反応式
[CH:1]1([N:4]2[C:13]3[C:8](=[CH:9][C:10]([F:17])=[C:11](F)[C:12]=3[O:14][CH3:15])[C:7](=[O:18])[C:6]([C:19]([OH:21])=[O:20])=[CH:5]2)[CH2:3][CH2:2]1.C([NH:29][CH2:30][CH2:31][NH2:32])(OC(C)(C)C)=O.FC(F)(F)C(O)=O>CN(C)C(=O)C.CO>[NH2:29][CH2:30][CH2:31][NH:32][C:11]1[C:12]([O:14][CH3:15])=[C:13]2[C:8]([C:7](=[O:18])[C:6]([C:19]([OH:21])=[O:20])=[CH:5][N:4]2[CH:1]2[CH2:3][CH2:2]2)=[CH:9][C:10]=1[F:17]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 6422Trifluoroacetic acidHCID 187201N-BOC-ethylenediamineHCID 70194651-Cyclopropyl-6,7-difluoro-1,4-dihydro-8-methoxy-4-oxo-3-quinolinecarboxylic acid

生成物 1

HCID 18448976Despropylene Gatifloxacin収率 58,848.5%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒
HCID 31374
Dimethylacetamide
溶媒

反応条件

温度
120 °C

実験手順

To a solution of 1-cyclopropyl-1,4-dihydro-4-oxo-6,7-difluoro-8-methoxy-3-quinoline carboxylic acid (1.0 g) in N,N-dimethylacetamide (10 ml), N-BOC-ethylenediamine (0.82 mg) was added. The mixture was heated at 120° C. for 12 h. Trifluoracetic acid (20 ml) was added and the reaction mixture was stirred at r.t. for 24 h. The solvent was evaporated under reduced pressure. The crude product was dissolved in water (5 ml) and pH adjusted with 20% NaOH to 7. The precipitate obtained was dispersed in MeOH and filtered to give the title compound (1.01 g).

後処理

  1. customThe solvent was evaporated under reduced pressure
  2. dissolutionThe crude product was dissolved in water (5 ml)
  3. customThe precipitate obtained
  4. filtrationfiltered

出典と根拠

ORDレコード
ord-28893d5a79ff45318058e6925aea518f
出典データセット
uspto-grants-2007_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07202221B2

反応ノート

読み込み中…

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