Ammonia → 8-Nitro-2,3,4,5-tetrahydro-1H-1-benzazepine
반응식
[NH:1]1[CH2:7][CH2:6][CH2:5][CH2:4][C:3]2[CH:8]=[CH:9][CH:10]=[CH:11][C:2]1=2.[N+:12]([O-])([O-:14])=[O:13].[K+].N>OS(O)(=O)=O>[N+:12]([C:10]1[CH:9]=[CH:8][C:3]2[CH2:4][CH2:5][CH2:6][CH2:7][NH:1][C:2]=2[CH:11]=1)([O-:14])=[O:13]참가 물질
5
실험 절차
At −10° C., 2,3,4,5-tetrahydro-1H-benzo[b]azepine (1.9 g, 13 mmol) was added dropwise to a solution of KNO3 (3 g, 30 mmol) in H2SO4 (50 mL). The mixture was stirred for 40 min, poured over crushed ice, basified with aq. ammonia to pH 13, and extracted with EtOAc. The combined organic phases were washed with brine, dried over Na2SO4 and concentrated to give 8-nitro-2,3,4,5-tetrahydro-1H-benzo[b]azepine as a black solid (1.3 g, 51%), which was used without further purification.
후처리
- additionpoured
- customover crushed ice
- extractionextracted with EtOAc
- washThe combined organic phases were washed with brine
- dry with materialdried over Na2SO4
- concentrationconcentrated
출처 및 근거
- ORD 기록
- ord-4408e440c14949c580c69743d4cbf49b
- 출처 데이터셋
- uspto-grants-2014_09
- 특허 번호
- US08829204B2
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