3-bromo-2-methoxy-5-methyl-6,7,8,9-tetrahydro-5H-pyrido[2,3-d]azepine → HCID 178430478, 화합물
반응식
[Br:1][C:2]1[C:13]([O:14]C)=[N:12][C:5]2[CH2:6][CH2:7][NH:8][CH2:9][CH:10]([CH3:11])[C:4]=2[CH:3]=1>Br>[Br:1][C:2]1[C:13]([OH:14])=[N:12][C:5]2[CH2:6][CH2:7][NH:8][CH2:9][CH:10]([CH3:11])[C:4]=2[CH:3]=1참가 물질
3
실험 절차
3-Bromo-2-methoxy-5-methyl-6,7,8,9-tetrahydro-5H-pyrido[2,3-d]azepine (152 mg, 414 μmol) in 48% aq. HBr (50 ml) was heated at reflux for 1 h. After neutralization with Na2CO3 and concentration in vacuo, the residue was purified by column chromatography and furnished 13.3 mg (13%) of 3-bromo-5-methyl-6,7,8,9-tetrahydro-5H-pyrido[2,3-d]azepin-2-ol. 1H-NMR (CDCl3) δ 7.68 (s, 1H), 3.08-2.77 (m, 7H), 1.26 (d, 3H) ppm.
후처리
- temperatureat reflux for 1 h
- concentrationAfter neutralization with Na2CO3 and concentration in vacuo
- customthe residue was purified by column chromatography
출처 및 근거
- ORD 기록
- ord-bd72a6b4ef25421492961fec7bb1051d
- 출처 데이터셋
- uspto-grants-2011_03
- 특허 번호
- US07897595B2
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