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Hydrogen Bromide → HCID 23284711、化合物

HRID 369268
ノート
印刷プレビュー

反応式

HRID 369268 の反応式
[Cl:1][C:2]1[C:3]([F:31])=[C:4]([F:30])[CH:5]=[C:6]2[C:11]=1[N:10]([C:12]1[CH:17]=[C:16]([O:18]C)[C:15]([F:20])=[CH:14][C:13]=1[N+:21]([O-:23])=[O:22])[CH:9]=[C:8]([C:24]([O:26]CC)=[O:25])[C:7]2=[O:29].Br>C(O)(=O)C>[Cl:1][C:2]1[C:3]([F:31])=[C:4]([F:30])[CH:5]=[C:6]2[C:11]=1[N:10]([C:12]1[CH:17]=[C:16]([OH:18])[C:15]([F:20])=[CH:14][C:13]=1[N+:21]([O-:23])=[O:22])[CH:9]=[C:8]([C:24]([OH:26])=[O:25])[C:7]2=[O:29]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 260Hydrogen BromideHCID 23284751HCID 23284751、化合物

生成物 1

HCID 23284711HCID 23284711、化合物収率 47.5%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

Ethyl 8-chloro-6,7-difluoro-1-(4-fluoro-5-methoxy-2-nitrophenyl)-4-oxo-1,4-dihydroquinoline-3-carboxylate (510 mg) was added to a mixed liquid (1:1, v/v; 5 ml) of 47% hydrobromic acid and acetic acid, aid the mixture was stirred and heated under reflux for 46 hours. The reaction mixture was concentrated under reduced pressure. A process of adding distilled water (5 ml) to the residue and then concentrating the mixture under reduced pressure was conducted twice repeatedly. Distilled water (5 ml) was added to the resultant residue, and deposits were collected by filtration. The deposits were dispersed in ethanol (2 ml) and heated to reflux. The reaction mixture was allowed to cool, and deposits were collected by filtration and washed with ethanol and diisopropyl ether in that order to obtain the title compound (220 mg) as a pale brown powder.

後処理

  1. temperatureheated
  2. temperatureunder reflux for 46 hours
  3. concentrationThe reaction mixture was concentrated under reduced pressure
  4. additionA process of adding
  5. distillationdistilled water (5 ml) to the residue
  6. concentrationconcentrating the mixture under reduced pressure
  7. additionDistilled water (5 ml) was added to the resultant residue, and deposits
  8. filtrationwere collected by filtration
  9. additionThe deposits were dispersed in ethanol (2 ml)
  10. temperatureheated to reflux
  11. temperatureto cool
  12. filtrationdeposits were collected by filtration
  13. washwashed with ethanol and diisopropyl ether in that order

出典と根拠

ORDレコード
ord-f363a2f591394bc98b350cec2c71c958
出典データセット
uspto-grants-2000_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06136823

反応ノート

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