反応式
[CH:1]([N:4]1[CH2:9][CH2:8][N:7]([C:10]([C:12]2[CH:17]=[CH:16][C:15]([CH2:18][N:19]3[CH2:24][CH2:23][O:22][CH2:21][CH2:20]3)=[CH:14][CH:13]=2)=[O:11])[CH2:6][CH2:5]1)([CH3:3])[CH3:2].[C:25]([OH:32])(=[O:31])/[CH:26]=[CH:27]\[C:28]([OH:30])=[O:29]>CCO>[C:25]([OH:32])(=[O:31])/[CH:26]=[CH:27]\[C:28]([OH:30])=[O:29].[C:25]([OH:32])(=[O:31])/[CH:26]=[CH:27]\[C:28]([OH:30])=[O:29].[CH:1]([N:4]1[CH2:9][CH2:8][N:7]([C:10]([C:12]2[CH:13]=[CH:14][C:15]([CH2:18][N:19]3[CH2:20][CH2:21][O:22][CH2:23][CH2:24]3)=[CH:16][CH:17]=2)=[O:11])[CH2:6][CH2:5]1)([CH3:3])[CH3:2]参加物
4
反応条件
- 温度
- 75 °C
実験手順
To a solution of (4-isopropyl-piperazin-1-yl)-(4-morpholin-4-ylmethyl -phenyl)-methanone (3.0 g, 9.05 mmol) in absolute EtOH (20 mL) was added, via an addition funnel, a solution of maleic acid (3.3 g, 19.8 mmol) in absolute EtOH (20 mL) over 10 min. The resulting suspension was stirred at room temperature for 15 min, at 75° C. for 30 min, and was then allowed to cool to room temperature for 15 h. The reaction mixture was cooled further to 0° C. and was then stirred for 2 h. The resulting precipitate was collected by suction filtration and washed with cold EtOH (20 mL). The wet solid was dried in a vacuum oven at 40° C. for 6 h to yield the title compound as crude material, as a white solid.
後処理
- temperatureto cool to room temperature for 15 h
- temperatureThe reaction mixture was cooled further to 0° C.
- stirringwas then stirred for 2 h
- filtrationThe resulting precipitate was collected by suction filtration
- washwashed with cold EtOH (20 mL)
- customThe wet solid was dried in a vacuum oven at 40° C. for 6 h
出典と根拠
- ORDレコード
- ord-f61cc33c144f484db6ec21ca0b119229
- 出典データセット
- uspto-grants-2010_06
- 特許番号
- US07728129B2
関連ノート
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