反応式
[NH2:1][C:2]1[CH:33]=[CH:32][C:5]([C:6]([N:8]([CH2:15][CH2:16][N:17]2[CH2:22][CH2:21][CH:20]([C:23](=[O:31])[C:24]3[CH:29]=[CH:28][C:27]([F:30])=[CH:26][CH:25]=3)[CH2:19][CH2:18]2)[C:9]2[CH:10]=[N:11][CH:12]=[CH:13][CH:14]=2)=[O:7])=[CH:4][CH:3]=1.N1C=CC=CC=1.[F:40][C:41]([F:46])([F:45])[C:42](O)=[O:43].C(=O)(O)[O-].[Na+]>C(Cl)Cl>[F:40][C:41]([F:46])([F:45])[C:42]([NH:1][C:2]1[CH:33]=[CH:32][C:5]([C:6]([N:8]([CH2:15][CH2:16][N:17]2[CH2:22][CH2:21][CH:20]([C:23](=[O:31])[C:24]3[CH:25]=[CH:26][C:27]([F:30])=[CH:28][CH:29]=3)[CH2:19][CH2:18]2)[C:9]2[CH:10]=[N:11][CH:12]=[CH:13][CH:14]=2)=[O:7])=[CH:4][CH:3]=1)=[O:43]参加物
反応物 4
生成物 1
試薬・触媒・溶媒 1
実験手順
4-Amino-N-{2-[4-(4-fluorobenzoyl)piperidino]ethyl}-N-(3-pyridyl)benzamide (229.3 mg, 0.51 mmol) was dissolved in methylene chloride (2.0 ml) to which were subsequently added pyridine (0.05 ml, 0.62 mmol) and anhydrous trifluoroacetic acid (0.09 ml, 0.64 mmol) at 0° C. After 3 hours of stirring at 0° C. to room temperature, the reaction solution was mixed with saturated sodium bicarbonate aqueous solution and extracted with chloroform. The resulting organic layer was washed with saturated sodium chloride aqueous solution and water in that order, and dried on anhydrous sodium sulfate. Thereafter, the solvent was removed by evaporation, and the resulting residue was purified by silica gel column chromatography (chloroform:methanol=20:1) to obtain 224.8 mg (81.2%) of the title compound in a light yellow powder form.
後処理
- customat 0° C
- extractionextracted with chloroform
- washThe resulting organic layer was washed with saturated sodium chloride aqueous solution and water in that order
- dry with materialdried on anhydrous sodium sulfate
- customThereafter, the solvent was removed by evaporation
- customthe resulting residue was purified by silica gel column chromatography (chloroform:methanol=20:1)
出典と根拠
- ORDレコード
- ord-83156c93ebe44f9b836d2b41d4fbb6ea
- 出典データセット
- uspto-grants-1998_03
- 特許番号
- US05728835
関連ノート
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