Methanol → HCID 178486902、化合物
反応式
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([NH2:9])[C:6]([N+:10]([O-])=O)=[CH:5][N:4]=1.[CH3:13]O>[Pd]>[CH3:1][O:2][C:3]1[N:4]=[CH:5][C:6]2[N:10]=[CH:13][NH:9][C:7]=2[CH:8]=1参加物
4
実験手順
A solution of 15.51 g of 2-methoxy-5-nitropyridin-4-amine (example E7) in 1.55 I methanol was treated with 4.65 g Pd/C (10% Pd) and hydrogenated for 12 h under atmospheric pressure. The reaction mixture was filtered through a plug of CELITE® (diatomaceous earth) and the filtrate was concentrated under vacuum. The resulting residue was treated with 181 ml formic acid and the mixture was refluxed for 50 h. The formic acid was distilled off and the residue was repeatedly purified by flash chromatography (neutral alumina oxide, ethyl acetate/methanol) to yield the title compound.
後処理
- filtrationThe reaction mixture was filtered through a plug of CELITE® (diatomaceous earth)
- concentrationthe filtrate was concentrated under vacuum
- additionThe resulting residue was treated with 181 ml formic acid
- temperaturethe mixture was refluxed for 50 h
- distillationThe formic acid was distilled off
- customthe residue was repeatedly purified by flash chromatography (neutral alumina oxide, ethyl acetate/methanol)
出典と根拠
- ORDレコード
- ord-27bcb2a5bc1c4039ac9641ce91c8049e
- 出典データセット
- uspto-grants-2012_09
- 特許番号
- US08273890B2
反応ノート
読み込み中…