Acetic Acid → Diisopropyl Ether

HRID 1415937노트

반응식

HRID 1415937 반응식
[Cl:1][C:2]1[N:11]=[C:10]2[C:5]([C:6](=[O:27])[C:7]([C:22]([O:24]CC)=[O:23])=[CH:8][N:9]2[C:12]2[CH:17]=[C:16]([NH:18][CH3:19])[C:15]([F:20])=[CH:14][C:13]=2[F:21])=[CH:4][C:3]=1[F:28].Cl.[C:30]([OH:33])(=O)[CH3:31].O.[CH2:35](O)C>>[CH:3]([O:33][CH:30]([CH3:31])[CH3:35])([CH3:4])[CH3:2].[Cl:1][C:2]1[N:11]=[C:10]2[C:5]([C:6](=[O:27])[C:7]([C:22]([OH:24])=[O:23])=[CH:8][N:9]2[C:12]2[CH:17]=[C:16]([NH:18][CH3:19])[C:15]([F:20])=[CH:14][C:13]=2[F:21])=[CH:4][C:3]=1[F:28]

참가 물질

7

반응물 5

HCID 176Acetic AcidHCID 313Hydrochloric AcidHCID 702EthanolHCID 962WaterHCID 54102467Ethyl 7-chloro-1-(2,4-difluoro-5-methylaminophenyl)-6-fluoro-1,4-dihydro-4-oxo-1,8-naphthyridine-3-carboxylate

생성물 2

HCID 7914Diisopropyl EtherHCID 224410407-Chloro-1-(2,4-difluoro-5-methylaminophenyl)-6-fluoro-1,4-dihydro-4-oxo-1,8-naphthyridine-3-carboxylic acid

실험 절차

Ethyl 7-chloro-1-(2,4-difluoro-5-methylaminophenyl)-6-fluoro-4-oxo-1,4-dihydro-1,8-naphthyridine-3-carboxylate (150 mg) was added to 1 ml of a mixture of 3N hydrochloric acid and acetic acid (1/1, vol/vol), which was stirred and heated at reflux for 2 hours. After 5 ml of distilled water was added, the reaction solution was heated at reflux for a further 10 minutes and then allowed to cool down. The precipitate was dispersed in ethanol, collected by filtration, and washed with ethanol and then with diisopropyl ether to give 70 mg of the title compound.

후처리

  1. temperatureheated
  2. temperatureat reflux for 2 hours
  3. temperaturethe reaction solution was heated
  4. temperatureat reflux for a further 10 minutes
  5. temperatureto cool down
  6. filtrationcollected by filtration
  7. washwashed with ethanol

출처 및 근거

ORD 기록
ord-b5f1180e84c64a09b1026431cbc4114a
출처 데이터셋
uspto-grants-1999_06
특허 번호
US05910498

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