反応式
[O-:1][CH2:2][CH3:3].[Na+].[Na].[CH:6]1([N:9]2[C:18]3[C:13](=[CH:14][C:15]([F:26])=[C:16]([N:20]4[CH2:25][CH2:24][NH:23][CH2:22][CH2:21]4)[C:17]=3F)[C:12](=[O:27])[C:11]([C:28]([OH:30])=[O:29])=[CH:10]2)[CH2:8][CH2:7]1>C(O)C>[CH:6]1([N:9]2[C:18]3[C:13](=[CH:14][C:15]([F:26])=[C:16]([N:20]4[CH2:21][CH2:22][NH:23][CH2:24][CH2:25]4)[C:17]=3[O:1][CH2:2][CH3:3])[C:12](=[O:27])[C:11]([C:28]([OH:30])=[O:29])=[CH:10]2)[CH2:7][CH2:8]1参加物
実験手順
To a solution of sodium ethoxide prepare from sodium (0.75 g) and absolute ethanol (30 ml) was added 1-cyclopropyl-6,8-difluoro-1,4-dihydro-4-oxo-7-(1-piperazinyl)-3-quinolinecarboxylic acid (0.8 g) and the mixture in sealed tube was stirred for 52 hours at 140° to 150° C. and then concentrated. Water (60 ml) was added to the residue, and the solution was adjusted pH 7 with acetic acid and and extracted with chloroform. The chloroform layer was washed with saturated saline solution, dried over anhydrous sodium sulfate and then concentrated. The resulting residue was purified by silica gel column chromatography eluting with chloroform-methanol (2:1)→chloroform-methanol-concentrated aqueous ammonia (20:6:1→10:10:1) and recrystallized from ethanol to give the title compound (75 mg) as light brown prisms, mp 119°-122° C.
後処理
- concentrationconcentrated
- additionWater (60 ml) was added to the residue
- extractionextracted with chloroform
- washThe chloroform layer was washed with saturated saline solution
- dry with materialdried over anhydrous sodium sulfate
- concentrationconcentrated
- customThe resulting residue was purified by silica gel column chromatography
- washeluting with chloroform-methanol (2:1)→chloroform-methanol-concentrated aqueous ammonia (20:6:1→10:10:1)
- customrecrystallized from ethanol
出典と根拠
- ORDレコード
- ord-9216f9bff4b8417d837377c818b3be8e
- 出典データセット
- uspto-grants-1990_12
- 特許番号
- US04980470
関連ノート
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