反応式
Cl.[Br:2][C:3]1[CH:4]=[C:5]([CH:8]=[CH:9][CH:10]=1)[CH2:6][NH2:7].[C:11](OC(=O)C)(=[O:13])[CH3:12].O.C(OCC)(=O)C>N1C=CC=CC=1>[Br:2][C:3]1[CH:4]=[C:5]([CH:8]=[CH:9][CH:10]=1)[CH2:6][NH:7][C:11](=[O:13])[CH3:12]参加物
6
実験手順
To a solution of 3-bromobenzylamine hydrochloride (5.20 g) in pyridine (30 ml) was added acetic anhydride (3.2 ml) at 0° C. and the mixture was stirred at room temperature for 24 h. Water and ethyl acetate were added to the reaction mixture for partitioning, and the organic layer was washed with 1N hydrochloric acid, aqueous sodium hydrogen carbonate and brine, dried (magnesium sulfate) and concentrated under reduced pressure. The residue was recrystallized from hexane-ethyl acetate to give the title compound (4.00 g) as colorless needle crystals.
後処理
- customfor partitioning
- washthe organic layer was washed with 1N hydrochloric acid, aqueous sodium hydrogen carbonate and brine
- dry with materialdried (magnesium sulfate)
- concentrationconcentrated under reduced pressure
- customThe residue was recrystallized from hexane-ethyl acetate
出典と根拠
- ORDレコード
- ord-35cf1564147845648b941737314ce4d1
- 出典データセット
- uspto-grants-2003_02
- 特許番号
- US06518257B1
関連ノート
読み込み中…