反応式
[CH2:1]([N:3]1[C:12]2[C:7](=[CH:8][C:9]([F:14])=[C:10](Cl)[CH:11]=2)[C:6](=[O:15])[C:5]([C:16]([OH:18])=[O:17])=[CH:4]1)[CH3:2].[OH2:19].O.O.O.O.O.[NH:25]1[CH2:30][CH2:29][NH:28][CH2:27][CH2:26]1>O>[OH2:15].[OH2:19].[OH2:15].[OH2:15].[OH2:15].[CH2:1]([N:3]1[C:12]2[C:7](=[CH:8][C:9]([F:14])=[C:10]([N:25]3[CH2:30][CH2:29][NH:28][CH2:27][CH2:26]3)[CH:11]=2)[C:6](=[O:15])[C:5]([C:16]([OH:18])=[O:17])=[CH:4]1)[CH3:2]参加物
4
反応条件
- 温度
- 170 °C
実験手順
A mixture of 1-ethyl-6-fluoro-7-chloro-1,4-dihydro-4-oxoquinoline-3-carboxylic acid (1.9g), piperazine hexahydrate (15g) and water (15 ml) was heated at 170° C. in a sealed tube for 16 hr. After evaporation of the solvent, the residue was acidified with diluted hydrochloric acid, heated at 100° C., and the hot solution was filtered. The filtrate was evaporated to dryness. The residue was dissolved in 10% sodium hydroxide and neutralized with acetic acid. The precipitate was collected, washed with water, dried, and recrystallized from ethanol to give 1-ethyl-6-fluoro-1,4-dihydro-7-(1-piperazinyl)-4-oxoquinoline-3-carboxylic acid pentahydrate (I) as colorless powder, m.p.: 226°-227° C. Mass spectrum m/e: 319 (M+).
後処理
- customAfter evaporation of the solvent
- temperatureheated at 100° C.
- filtrationthe hot solution was filtered
- customThe filtrate was evaporated to dryness
- dissolutionThe residue was dissolved in 10% sodium hydroxide and neutralized with acetic acid
- customThe precipitate was collected
- washwashed with water
- customdried
- customrecrystallized from ethanol
出典と根拠
- ORDレコード
- ord-3f951248f3f94041966d29418c103210
- 出典データセット
- uspto-grants-1979_03
- 特許番号
- US04146719
関連ノート
読み込み中…