Sodium Hydroxide → Magnesium [5-amino-1-cyclopropyl-8-difluoromethoxy-6-fluoro-7-(3-methylpiperazinyl)-1,4-dihydro-4-oxoquinoline-3-carboxylate]
反応式
[OH-].[Na+].[NH2:3][C:4]1[C:13]([F:14])=[C:12]([N:15]2[CH2:20][CH2:19][NH:18][CH:17]([CH3:21])[CH2:16]2)[C:11]([O:22][CH:23]([F:25])[F:24])=[C:10]2[C:5]=1[C:6](=[O:32])[C:7]([C:29]([OH:31])=[O:30])=[CH:8][N:9]2[CH:26]1[CH2:28][CH2:27]1.[Cl-].[Mg+2:34].[Cl-]>>[NH2:3][C:4]1[C:13]([F:14])=[C:12]([N:15]2[CH2:20][CH2:19][NH:18][CH:17]([CH3:21])[CH2:16]2)[C:11]([O:22][CH:23]([F:24])[F:25])=[C:10]2[C:5]=1[C:6](=[O:32])[C:7]([C:29]([O-:31])=[O:30])=[CH:8][N:9]2[CH:26]1[CH2:27][CH2:28]1.[Mg+2:34].[NH2:3][C:4]1[C:13]([F:14])=[C:12]([N:15]2[CH2:20][CH2:19][NH:18][CH:17]([CH3:21])[CH2:16]2)[C:11]([O:22][CH:23]([F:24])[F:25])=[C:10]2[C:5]=1[C:6](=[O:32])[C:7]([C:29]([O-:31])=[O:30])=[CH:8][N:9]2[CH:26]1[CH2:27][CH2:28]1参加物
反応物 3
生成物 1
実験手順
23.0 ml (0.0023 mole) of a 0.1N aqueous solution of sodium hydroxide were added to 1.00 g (0.00234 mole) of 5-amino-1-cyclopropyl-8-difluoromethoxy-6-fluoro-7-(3-methylpiperazinyl)-1,4-dihydro-4-oxoquinoline-3-carboxylic acid (prepared as described in Example 30), and the resulting insoluble material was removed by filtration. 0.11 g (0.00115 mole) of anhydrous magnesium chloride was added to the filtrate, and the mixture was stirred at room temperature for 90 minutes. At the end of this time, the resulting precipitate was collected by filtration and washed with water, to give 0.91 g of magnesium [5-amino-1-cyclopropyl-8-difluoromethoxy-6-fluoro-7-(3-methylpiperazinyl)-1,4-dihydro-4-oxoquinoline-3-carboxylate] as a yellow powder, melting at 291°-293° C. (with decomposition).
後処理
- customthe resulting insoluble material was removed by filtration
- filtrationAt the end of this time, the resulting precipitate was collected by filtration
- washwashed with water
出典と根拠
- ORDレコード
- ord-8b7358fe8c3545a9b74de81ac4ba56a3
- 出典データセット
- uspto-grants-1996_03
- 特許番号
- US05496951
反応ノート
読み込み中…