Benzoic acid, 4-amino-3-nitro- → 4-Amino-3-bromo-5-nitrobenzoic acid
反応式
[NH2:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[CH:4][C:3]=1[N+:11]([O-:13])=[O:12].[Br:14]NC(=O)CCC(N)=O>ClCCl.CN(C)C=O>[NH2:1][C:2]1[C:3]([N+:11]([O-:13])=[O:12])=[CH:4][C:5]([C:6]([OH:8])=[O:7])=[CH:9][C:10]=1[Br:14]参加物
5
実験手順
To a solution of 4-amino-3-nitrobenzoic acid (2.50 g, 13.7 mmol) in dichloromethane (65.4 mL) and N,N-dimethylformamide (3.3 mL) was added N-bromosuccinamide (2.69 g, 15.1 mmol). The mixture was stirred at ambient temperature. After 15 min, the mixture was quenched with saturated sodium sulfite. Hydrochloric acid (1.0 M) was added and the mixture was extracted with dichloromethane. The combined organic layer was washed with brine, dried over magnesium sulfate, filtered and concentrated (3.65 g). LC-MS [M]=261.0.
後処理
- customthe mixture was quenched with saturated sodium sulfite
- additionHydrochloric acid (1.0 M) was added
- extractionthe mixture was extracted with dichloromethane
- washThe combined organic layer was washed with brine
- dry with materialdried over magnesium sulfate
- filtrationfiltered
- concentrationconcentrated (3.65 g)
出典と根拠
- ORDレコード
- ord-bd61b728cc4b485bba95427f26a8d8f8
- 出典データセット
- uspto-grants-2016_01
- 特許番号
- US09238647B2
反応ノート
読み込み中…