反応式
[Cl:1][C:2]1[C:3](F)=[C:4]([F:19])[CH:5]=[C:6]2[C:11]=1[N:10]([CH:12]1[CH2:14][CH2:13]1)[CH:9]=[C:8]([C:15]([OH:17])=[O:16])[C:7]2=[O:18].[N:21]1([CH2:28][CH2:29][OH:30])[CH2:27][CH2:26][CH2:25][NH:24][CH2:23][CH2:22]1>N1C=CC=CC=1>[Cl:1][C:2]1[C:3]([N:24]2[CH2:25][CH2:26][CH2:27][N:21]([CH2:28][CH2:29][OH:30])[CH2:22][CH2:23]2)=[C:4]([F:19])[CH:5]=[C:6]2[C:11]=1[N:10]([CH:12]1[CH2:14][CH2:13]1)[CH:9]=[C:8]([C:15]([OH:17])=[O:16])[C:7]2=[O:18]参加物
反応物 2
生成物 1
試薬・触媒・溶媒 1
実験手順
350 mg (1.2 mmol) of 8-Chloro-1-cyclopropyl-6,7-difluoro-4-oxo-1,4-dihydroquinoline-3-carboxylic acid (for preparation see: DE 3420743) are dissolved according to DE 3635218 in 3 ml of dry pyridine and heated at reflux with 202 mg (1.4 mmol) of hexahydro-1H-1,4-diazepine-1-ethanol for 4 hours. After standing overnight the mixture is concentrated, taken up with water and brought to pH 6 using dilute hydrochloric acid. The solution is saturated with sodium chloride at boiling heat. After it has cooled to room temperature, it is extracted a number of times with dichloromethane. The organic extracts are filtered over a little silica gel and concentrated. 288 mg of the target compound are obtained this way. The compound is used as a crude product in the subsequent reaction stages.
後処理
- temperatureheated
- concentrationthe mixture is concentrated
- temperatureat boiling heat
- extractionit is extracted a number of times with dichloromethane
- filtrationThe organic extracts are filtered over a little silica gel
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-1cb32486c03048e2a61c9a4e78e3af14
- 出典データセット
- uspto-grants-2011_01
- 特許番号
- US07867992B2
関連ノート
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