Sodium hydride → Moxifloxacin difluoro methoxy ethyl ester

HRID 1770111

反応式

HRID 1770111 の反応式
[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]

参加物

4

反応物 2

HCID 24758Sodium hydrideHCID 178471878HCID 178471878、化合物

生成物 1

HCID 10758239Moxifloxacin difluoro methoxy ethyl ester収率 75%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
50 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-5d49d6c7b08743c19637ed2231c32785
出典データセット
uspto-grants-1995_01
特許番号
US05385913

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