Sodium hydride → Moxifloxacin difluoro methoxy ethyl ester

HRID 1770111

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HRID 1770111 반응식
[CH3:1][O:2][C:3]1[C:4](F)=[C:5]([CH:19]=[C:20]([F:23])[C:21]=1[F:22])[C:6]([C:8](=[CH:14][NH:15][CH:16]1[CH2:18][CH2:17]1)[C:9]([O:11][CH2:12][CH3:13])=[O:10])=[O:7].[H-].[Na+]>O1CCCC1>[CH3:1][O:2][C:3]1[C:21]([F:22])=[C:20]([F:23])[CH:19]=[C:5]2[C:4]=1[N:15]([CH:16]1[CH2:18][CH2:17]1)[CH:14]=[C:8]([C:9]([O:11][CH2:12][CH3:13])=[O:10])[C:6]2=[O:7]

참가 물질

4

반응물 2

HCID 24758Sodium hydrideHCID 178471878HCID 178471878, 화합물

생성물 1

HCID 10758239Moxifloxacin difluoro methoxy ethyl ester수율 75%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
50 °C

실험 절차

To a solution of ethyl 2-(3-methoxy-2,4,5-trifluorobenzoyl)-3-cyclopropylaminoacrylate (440 mg, 1.29 mmol) in anhydrous tetrahydrofuran (15 mL) at 0° C. was added sodium hydride (62 mg, 1.5 mmol, 1.1 equiv, 60% in mineral oil). The reaction mixture was allowed to stir at 50° C. for 12 hours. The mixture was cooled to room temperature and filtered. The mother liquor was concentrated and a white precipitate formed. The material was collected by suction filtration and air-dried to give 312 mg, 75% yield of a pure white solid, m.p. 178°-181° C.

후처리

  1. temperatureThe mixture was cooled to room temperature
  2. filtrationfiltered
  3. concentrationThe mother liquor was concentrated
  4. customa white precipitate formed
  5. filtrationThe material was collected by suction filtration
  6. customair-dried

출처 및 근거

ORD 기록
ord-5d49d6c7b08743c19637ed2231c32785
출처 데이터셋
uspto-grants-1995_01
특허 번호
US05385913

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