Water → 1-(1-Amino-1H-pyrrol-2-yl)ethanone
反応式
[C:1]([C:4]1[N:5]([N:9]2C(=O)C3C(=CC=CC=3)C2=O)[CH:6]=[CH:7][CH:8]=1)(=[O:3])[CH3:2].CN.O>CN(C)C=O>[NH2:9][N:5]1[CH:6]=[CH:7][CH:8]=[C:4]1[C:1](=[O:3])[CH3:2]参加物
5
実験手順
To a suspension of 2-(2-acetyl-1H-pyrrol-1-yl)-1H-isoindole-1,3(2H)dione (8.53 g) in dimethylformamide (25 ml) was added 33 ml of 40% methylamine solution. After 2.5 hours, the reaction mixture was poured into water (300 ml) and was extracted 4 times with EtOAc. The combined organics were washed once with water and brine, dried (MgSO4), filtered and concentrated to give the crude product. Purification via flash column chromatography (silica gel, 30% EtOAc/hexane) afforded 3.88 g of the product as an oil.
後処理
- extractionwas extracted 4 times with EtOAc
- washThe combined organics were washed once with water and brine
- dry with materialdried (MgSO4)
- filtrationfiltered
- concentrationconcentrated
- customto give the crude product
- customPurification via flash column chromatography (silica gel, 30% EtOAc/hexane)
出典と根拠
- ORDレコード
- ord-b14709ea61d846a78180e562f3dadce8
- 出典データセット
- uspto-grants-1997_02
- 特許番号
- US05605925
反応ノート
読み込み中…