Hydrochloric Acid → Anthranilamide
反応式
Cl.[N+:2]([C:5]1[CH:13]=[CH:12][CH:11]=[CH:10][C:6]=1[C:7]([NH2:9])=[O:8])([O-])=O.C(=O)([O-])[O-].[Na+].[Na+]>CO.[Fe]>[NH2:2][C:5]1[CH:13]=[CH:12][CH:11]=[CH:10][C:6]=1[C:7]([NH2:9])=[O:8]参加物
6
反応条件
- 温度
- 80 °C
実験手順
Concentrated hydrochloric acid (140μL) was added to a solution of the nitrobenzamide, V.3 (147 mg, 0.30 mmol) in methanol (2 ml). Iron (72 mg) was added and the reaction mixture was heated to 80° C. for 2 hours, before cooling. The reaction mixture was basified (saturated sodium carbonate solution), extracted into ethyl acetate, dried over magnesium sulphate and the solvent removed in vacuo to yield an off-white solid which was purified using flash chromatography(ethyl acetate) to yield the desired 2-aminobenzamide, VI.3 (47 mg, 34%).
後処理
- temperaturebefore cooling
- extractionextracted into ethyl acetate
- dry with materialdried over magnesium sulphate
- customthe solvent removed in vacuo
- customto yield an off-white solid which
- customwas purified
出典と根拠
- ORDレコード
- ord-26babed926144b1b90eb38edd92a4e13
- 出典データセット
- uspto-grants-2001_04
- 特許番号
- US06218393B1
反応ノート
読み込み中…