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Hydrogen Bromide → HCID 23284711, 화합물

HRID 369268
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HRID 369268 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 260Hydrogen BromideHCID 23284751HCID 23284751, 화합물

생성물 1

HCID 23284711HCID 23284711, 화합물수율 47.5%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-f363a2f591394bc98b350cec2c71c958
출처 데이터셋
uspto-grants-2000_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06136823

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