反応式
[Cl:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[CH:5]=[C:4]([C:12]2[CH:17]=[CH:16][C:15]([O:18][CH3:19])=[CH:14][CH:13]=2)[N:3]=1.[CH2:20]([CH:22]1[CH2:27][CH2:26][NH:25][CH2:24][CH2:23]1)[CH3:21].C(N(CC)CC)C>CN(C)C=O>[ClH:1].[CH2:20]([CH:22]1[CH2:27][CH2:26][N:25]([C:2]2[C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[CH:5]=[C:4]([C:12]3[CH:17]=[CH:16][C:15]([O:18][CH3:19])=[CH:14][CH:13]=3)[N:3]=2)[CH2:24][CH2:23]1)[CH3:21]参加物
5
反応条件
- 温度
- 80 °C
実験手順
1-Chloro-3-(4-methoxyphenyl)isoquinoline (405 mg) and 4-ethylpiperidine (168 mg) were dissolved in N,N-dimethylformamide (5 ml), followed by the addition of triethylamine (251 ml), and the mixture was stirred at 80° C. overnight. The reaction mixture was partitioned between ethyl acetate and water. The resulting organic layer was washed with water, dried (over MgSO4) and evaporated. The resulting residue was purified by silica gel column chromatography (ethyl acetate/hexane system). Then the resulting product was converted into a hydrochloride in a conventional manner, and then recrystallized from ethanol/isopropyl ether, to give the hydrochloride of the title compound as a colorless crystals (87 mg, yield; 13%).
後処理
- customThe reaction mixture was partitioned between ethyl acetate and water
- washThe resulting organic layer was washed with water
- dry with materialdried (over MgSO4)
- customevaporated
- customThe resulting residue was purified by silica gel column chromatography (ethyl acetate/hexane system)
- customrecrystallized from ethanol/isopropyl ether
出典と根拠
- ORDレコード
- ord-c2af1ab155824703bebf4cabb2f0d6e2
- 出典データセット
- uspto-grants-2004_09
- 特許番号
- US06790844B2
関連ノート
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