反応式
[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=2[O:14][CH3:15])[CH2:4][CH2:3]1.[Cl:16][S:17](O)(=[O:19])=[O:18].C(=O)([O-])[O-].[Na+].[Na+].CC1C=CC(COC(NNC(C2C=NC=CN=2)=O)=O)=CC=1>ClCCl>[CH3:1][N:2]1[CH2:3][CH2:4][N:5]([C:8]2[CH:13]=[C:12]([S:17]([Cl:16])(=[O:19])=[O:18])[CH:11]=[CH:10][C:9]=2[O:14][CH3:15])[CH2:6][CH2:7]1参加物
6
反応条件
- 温度
- 0 °C
実験手順
2-(4-Methylpiperazin-1-yl)anisole (200 mg, 1 mmol) was added in portions over ten minutes to ice-cooled, stirred chlorosulfonic acid (1.2 ml) under argon. The resulting brown solution was stirred at 0° C. for 0.25 h and then at ambient temperature for a further 1.25 h. The solution was slowly poured onto crushed ice (50 g). Dichloromethane (50 ml) was added to the mixture followed by saturated sodium carbonate solution until pH10 was attained in the aqueous phase. The layers were separated and the aqueous phase further extracted with dicholoromethane. The combined organic phases were dried (Na2SO4) and concentrated to an oil. The oil was stirred with hexane (4 ml) to give the title compound as a cream solid (210 mg, 71%).
後処理
- temperaturecooled
- waitat ambient temperature for a further 1.25 h
- additionThe solution was slowly poured
- customThe layers were separated
- extractionthe aqueous phase further extracted with dicholoromethane
- dry with materialThe combined organic phases were dried (Na2SO4)
- concentrationconcentrated to an oil
- stirringThe oil was stirred with hexane (4 ml)
出典と根拠
- ORDレコード
- ord-a7c8edddd4ed45baa46af733d2f932a9
- 出典データセット
- uspto-grants-2001_11
- 特許番号
- US06316450B1
関連ノート
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