Dimethylformamide → 5-nitro-3,4-dihydro-2H-1,4-benzoxazin-3-one
反応式
[NH2:1][C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[CH:6][CH:5]=[CH:4][C:3]=1[OH:11].Br[CH2:13][C:14](OCC)=[O:15].C(=O)([O-])[O-].[K+].[K+].CN(C=O)C>O>[N+:8]([C:7]1[C:2]2[NH:1][C:14](=[O:15])[CH2:13][O:11][C:3]=2[CH:4]=[CH:5][CH:6]=1)([O-:10])=[O:9]参加物
6
実験手順
A mixture of 2-amino-3-nitrophenol (1.54 g, 10 mmol), ethyl bromoacetate (1.67 g, 10 mmol), potassium carbonate (1.54 g, 11 mmol) and DMF (5.0 mL) was stirred at room temperature for 20 h. Reaction mixture was diluted with water (100 mL) and extracted with ethyl acetate (100 mL×3). Combined ethyl acetate layers were washed with water (50 mL×2), dried (brine, sodium sulphate), concentrated and dried on high vacuum to give 5-Nitro-4H-benzo[1,4]oxazin-3-one, K-64 (1.6 g).
後処理
- customReaction mixture
- extractionextracted with ethyl acetate (100 mL×3)
- washCombined ethyl acetate layers were washed with water (50 mL×2)
- dry with materialdried (brine, sodium sulphate)
- concentrationconcentrated
- customdried on high vacuum
出典と根拠
- ORDレコード
- ord-b4fca33ea2a6468594c6b58979435362
- 出典データセット
- uspto-grants-2010_05
- 特許番号
- US07714017B2
反応ノート
読み込み中…