Ammonia → 2-Bromo-4,6-dinitroaniline
反応式
O.[N+:2]([C:5]1[CH:11]=[C:10]([N+:12]([O-:14])=[O:13])[CH:9]=[CH:8][C:6]=1[NH2:7])([O-:4])=[O:3].[Br:15]Br.N>C(O)(=O)C>[Br:15][C:8]1[CH:9]=[C:10]([N+:12]([O-:14])=[O:13])[CH:11]=[C:5]([N+:2]([O-:4])=[O:3])[C:6]=1[NH2:7]参加物
6
実験手順
To a stirred mixture of water (3.75 L) and acetic acid (375 mL) at rt was added 2,4-dinitroaniline (500 g, 2.73 mol) followed by dropwise addition of bromine (210 mL, 4.09 mol) over 30 min. The reaction mixture was stirred at rt for 15 min then heated to 100° C. for 2 h. The reaction mixture was then cooled to rt poured onto ice-cold water (5-6 L) and basified (pH 8-10) with aqueous ammonia. The solid thus obtained was filtered, washed with cold water and dried under vacuum. The resulting solid was washed with n-pentane to give the desired product (600 g, 84%).
後処理
- temperaturethen heated to 100° C. for 2 h
- temperatureThe reaction mixture was then cooled to rt
- additionpoured onto ice-cold water (5-6 L)
- customThe solid thus obtained
- filtrationwas filtered
- washwashed with cold water
- customdried under vacuum
- washThe resulting solid was washed with n-pentane
出典と根拠
- ORDレコード
- ord-0bbc4b2c48de4f10b61d6400c7c470a2
- 出典データセット
- uspto-grants-2015_11
- 特許番号
- US09181234B2
反応ノート
読み込み中…