反応式
Cl[C:2]1[CH:11]=[CH:10][C:9]2[C:4](=[CH:5][CH:6]=[C:7]([N+:12]([O-:14])=[O:13])[CH:8]=2)[N:3]=1.[NH:15]1[CH2:20][CH2:19][CH2:18][CH2:17][CH2:16]1>C(O)C>[N+:12]([C:7]1[CH:8]=[C:9]2[C:4](=[CH:5][CH:6]=1)[N:3]=[C:2]([N:15]1[CH2:20][CH2:19][CH2:18][CH2:17][CH2:16]1)[CH:11]=[CH:10]2)([O-:14])=[O:13]参加物
4
実験手順
The product (208 mg, 1.0 mmol) from Step B and piperidine (0.5 mL, 5 mmol) were mixed in absolute ethanol (3 mL) and then heated at reflux for 4 h. The reaction mixture was cooled to r.t., and the solvent removed under vacuum. The solids were taken up in EtOAc (125 mL). The mixture was transferred to a separatory funnel and washed with water (3×15 mL). The organic layer was dried over sodium sulfate, filtered and the solvent removed under vacuum to afford the product as a yellow solid, MS: m/z 258 (MH+) which was used without further purification.
後処理
- temperatureheated
- temperatureat reflux for 4 h
- customthe solvent removed under vacuum
- customThe mixture was transferred to a separatory funnel
- washwashed with water (3×15 mL)
- dry with materialThe organic layer was dried over sodium sulfate
- filtrationfiltered
- customthe solvent removed under vacuum
出典と根拠
- ORDレコード
- ord-0a730dd69aee4455b345209e15cac609
- 出典データセット
- uspto-grants-2006_08
- 特許番号
- US07084156B2
関連ノート
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