3-bromo-2-methoxy-5-methyl-6,7,8,9-tetrahydro-5H-pyrido[2,3-d]azepine → HCID 178430478、化合物
反応式
[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]=1参加物
3
実験手順
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.
後処理
- temperatureat reflux for 1 h
- concentrationAfter neutralization with Na2CO3 and concentration in vacuo
- customthe residue was purified by column chromatography
出典と根拠
- ORDレコード
- ord-bd72a6b4ef25421492961fec7bb1051d
- 出典データセット
- uspto-grants-2011_03
- 特許番号
- US07897595B2
反応ノート
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