反応式
[N+:1]([C:4]1[CH:18]=[CH:17][CH:16]=[CH:15][C:5]=1[C:6]([N:8]1[CH:12]=[CH:11][CH:10]=[C:9]1[CH:13]=O)=[O:7])([O-])=O>C(OCC)(=O)C.Cl.[Pd]>[CH:10]1[CH:11]=[CH:12][N:8]2[C:6](=[O:7])[C:5]3[CH:15]=[CH:16][CH:17]=[CH:18][C:4]=3[NH:1][CH2:13][C:9]=12参加物
5
実験手順
A mixture of 1.5 g of N-(2-nitrobenzoyl)pyrrole-2-carboxaldehyde in 50 ml of ethyl acetate, 2 drops of concentrated HCl and 0.3 g of 10% Pd/C is shaken in a Parr apparatus under hydrogen pressure for 1.75 hours. The mixture is filtered, 0.4 g of 10% Pd/C added and the mixture shaken in a Parr apparatus under hydrogen pressure for 2 hours. The reaction mixture is filtered through diatomaceous earth and the filtrate concentrated in vacuo to give 1.0 g of a yellow oil. The residue is purified on thick layer chromatography plates by elution with 4:1 ethyl acetate:hexane to give 107 mg of the desired product as an oily solid.
後処理
- filtrationThe mixture is filtered
- addition0.4 g of 10% Pd/C added
- stirringthe mixture shaken in a Parr apparatus under hydrogen pressure for 2 hours
- filtrationThe reaction mixture is filtered through diatomaceous earth
- concentrationthe filtrate concentrated in vacuo
出典と根拠
- ORDレコード
- ord-8181dc70744b436dad248a360da37cc2
- 出典データセット
- uspto-grants-1996_05
- 特許番号
- US05516774
関連ノート
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