反応式
[CH:1]1([N:4]2[C:13]3[C:8](=[CH:9][C:10]([F:21])=[C:11]([N:15]4[CH2:20][CH2:19][NH:18][CH2:17][CH2:16]4)[C:12]=3[F:14])[C:7](=[O:22])[C:6]([C:23]([OH:25])=[O:24])=[CH:5]2)[CH2:3][CH2:2]1.[CH:26]([I:29])([CH3:28])[CH3:27].C(N(CC)CC)C>CN(C)C=O>[IH:29].[CH:1]1([N:4]2[C:13]3[C:8](=[CH:9][C:10]([F:21])=[C:11]([N:15]4[CH2:16][CH2:17][N:18]([CH:26]([CH3:28])[CH3:27])[CH2:19][CH2:20]4)[C:12]=3[F:14])[C:7](=[O:22])[C:6]([C:23]([OH:25])=[O:24])=[CH:5]2)[CH2:2][CH2:3]1参加物
5
反応条件
- 温度
- 80 °C
実験手順
A mixture of 3.5 g (0.01 mol) of 1-cyclopropyl-6,8-difluoro- 7-(piperazin-1-yl)-1,4-dihydro-4-oxoquinoline-3-carboxylic acid, 3.4 g (0.02 mol) of isopropyl iodide and 2.1 (0.02 mol) of triethylamine in 50 ml of dimethylformamide is heated to 80° C. in the course of 6 hours. After the solvent has been evaporated off, the residue is stirred with 30 ml of water and is then filtered off under suction, washed with water and recrystallised from methanol. 2.3 g of 1-cyclopropyl-6,8-difluoro-7-(4-isopropylpiperazin-1-yl)-1,4-dihydro-4-oxoquinoline-3-carboxylic acid hydriodide having a decomposition temperature of 306°-308° C. are obtained.
後処理
- customAfter the solvent has been evaporated off
- filtrationis then filtered off under suction
- washwashed with water
- customrecrystallised from methanol
出典と根拠
- ORDレコード
- ord-fbee618d44bd46c1800ec70fddfb1999
- 出典データセット
- uspto-grants-1985_12
- 特許番号
- US04556658
関連ノート
読み込み中…