反応式
CC(C)([O-])C.[K+].[Cl:7][C:8]1[CH:16]=[C:15]2[C:11]([CH:12]=[CH:13][NH:14]2)=[CH:10][CH:9]=1.[C:17]([N:20]1[CH2:29][C:28]([CH3:31])([CH3:30])[C:27]2[C:22](=[CH:23][C:24]([S:32](Cl)(=[O:34])=[O:33])=[CH:25][CH:26]=2)[CH2:21]1)(=[O:19])[CH3:18].C(OCC)(=O)C>O1CCCC1.O>[Cl:7][C:8]1[CH:16]=[C:15]2[C:11]([CH:12]=[CH:13][N:14]2[S:32]([C:24]2[CH:23]=[C:22]3[C:27]([C:28]([CH3:31])([CH3:30])[CH2:29][N:20]([C:17](=[O:19])[CH3:18])[CH2:21]3)=[CH:26][CH:25]=2)(=[O:33])=[O:34])=[CH:10][CH:9]=1参加物
反応物 4
生成物 1
試薬・触媒・溶媒 2
実験手順
Potassium tert-butoxide (37 mg, 0.33 mmol) was added to a stirred solution of 6-chloroindole (50 mg, 0.33 mmol) in dry tetrahydrofuran (1 ml) under argon at room temperature. After stirring for 5 minutes, a solution of 2-acetyl-4,4-dimethyl-1,2,3,4-tetrahydro-isoquinoline-7-sulfonyl chloride (D3) (100 mg, 0.33 mmol) in dry tetrahydrofuran (1 ml) was added and the solution was stirred for a further 3 h. Ethyl acetate (5 ml) and water (5 ml) were added to the reaction mixture, which was then shaken. The layers were separated and the organic phase was washed with brine (5 ml), dried (MgSO4) and concentrated in vacuo to an oil. The oil was purified by column chromatography over silica gel eluting with a gradient of acetone/toluene to afford the title compound (D4) (70 mg, 51%), MS: m/z (MH+) 417/419.
後処理
- stirringthe solution was stirred for a further 3 h
- stirringwas then shaken
- customThe layers were separated
- washthe organic phase was washed with brine (5 ml)
- dry with materialdried (MgSO4)
- concentrationconcentrated in vacuo to an oil
- customThe oil was purified by column chromatography over silica gel eluting with a gradient of acetone/toluene
出典と根拠
- ORDレコード
- ord-a915c780e31247d2aa26832773c9cdd8
- 出典データセット
- uspto-grants-2005_02
- 特許番号
- US06849644B2
関連ノート
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