反応式
[CH3:1][N:2]1[CH:6]=[C:5]([N+:7]([O-])=O)[CH:4]=[C:3]1[C:10]([NH:12][CH2:13][CH2:14][N:15]1[CH2:20][CH2:19][O:18][CH2:17][CH2:16]1)=[O:11].[CH3:21][N:22]1[CH:26]=[C:25]([N+:27]([O-:29])=[O:28])[CH:24]=[C:23]1[C:30](Cl)=[O:31]>CO.C(Cl)Cl.[Pd]>[CH3:1][N:2]1[CH:6]=[C:5]([NH:7][C:30]([C:23]2[N:22]([CH3:21])[CH:26]=[C:25]([N+:27]([O-:29])=[O:28])[CH:24]=2)=[O:31])[CH:4]=[C:3]1[C:10]([NH:12][CH2:13][CH2:14][N:15]1[CH2:20][CH2:19][O:18][CH2:17][CH2:16]1)=[O:11]参加物
6
反応物 2
生成物 1
試薬・触媒・溶媒 3
反応条件
- 温度
- 0 °C
実験手順
1-Methyl-N-[2-(4-morpholinyl)ethyl]-4-nitro-1H-pyrrole-2-carboxamide (1.42 g, 3.41 mmol; see step (iii) above) was dissolved in methanol (10 mL) and cooled to 0° C., Pd/C (0.055 g) was then added in small portions and the solution stirred under H2 for 3 h. The solution was then filtered and the solvent removed under reduced pressure. A solution of 1-methyl-4-nitro-1H-pyrrole-2-carbonyl chloride (0.642 g, 3.42 mmol) in DCM (10 mL) was added and the mixture allowed to stir for 1 h at RT. The solvent was then removed under reduced pressure and the crude product was separated on basified silica using a 1:1 solution of methanol ethyl acetate to yield the sub-title compound.
後処理
- filtrationThe solution was then filtered
- customthe solvent removed under reduced pressure
- stirringto stir for 1 h at RT
- customThe solvent was then removed under reduced pressure
- customthe crude product was separated on basified silica using a 1:1 solution of methanol ethyl acetate
出典と根拠
- ORDレコード
- ord-60e0de94851d488a89d4953e9735e5ba
- 出典データセット
- uspto-grants-2011_09
- 特許番号
- US08012967B2
関連ノート
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