Benzoic acid, 4-amino-3-nitro- → 4-Amino-3-bromo-5-nitrobenzoic acid
반응식
[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]참가 물질
5
실험 절차
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.
후처리
- 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)
출처 및 근거
- ORD 기록
- ord-bd61b728cc4b485bba95427f26a8d8f8
- 출처 데이터셋
- uspto-grants-2016_01
- 특허 번호
- US09238647B2
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