反応式
[O:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[CH2:6][NH:7][S:8]([C:11]1[CH:12]=[C:13]2[C:17](=[CH:18][CH:19]=1)[NH:16][C:15](=[O:20])[C:14]2=O)(=[O:10])=[O:9].[N+:22]([C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][C:26]=1[NH:31][NH2:32])([O-:24])=[O:23]>Cl.C(O)C>[O:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[CH2:6][NH:7][S:8]([C:11]1[CH:12]=[C:13]2[C:17](=[CH:18][CH:19]=1)[NH:16][C:15](=[O:20])[C:14]2=[N:32][NH:31][C:26]1[CH:27]=[CH:28][CH:29]=[CH:30][C:25]=1[N+:22]([O-:24])=[O:23])(=[O:10])=[O:9]参加物
5
反応条件
- 温度
- 120 °C
実験手順
A mixture of rpm161 (0.040 g, 0.114 mmol) 2-nitrophenylhydrazine (0.021 g, 0.126 mmol, 1.1 eq) and HCl (aq 4 M, 2 drops) in ethanol (3 mL) was heated in the CEM microwave at 120° C. for 15 min. After cooling to room temperature, pure product rpm168 was collected as an orange precipitate by filtration and dried in vacuo. The pure compound rpm168 was obtained without further purification (0.048 g, 0.099 mmol, 86%). MS (API-ES): m/z 459 (M+NH4)+; HRMS (API-ES) m/z Found: 459.1082 (M+NH4)+.
後処理
- temperatureAfter cooling to room temperature
- filtrationwas collected as an orange precipitate by filtration
- customdried in vacuo
- customwas obtained without further purification (0.048 g, 0.099 mmol, 86%)
出典と根拠
- ORDレコード
- ord-3013d6af1a784f6da467cae0cdc17c3c
- 出典データセット
- uspto-grants-2015_03
- 特許番号
- US08987474B2
関連ノート
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