反応式
[C:1]([NH:5][C:6](=[O:27])[CH2:7][N:8]1[C:14]2[CH:15]=[CH:16][CH:17]=[CH:18][C:13]=2[CH:12]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[CH2:11][CH:10](Br)[C:9]1=[O:26])([CH3:4])([CH3:3])[CH3:2].CN(C)C=O.[N-:33]=[N+:34]=[N-:35].[Na+].O>C(OCC)(=O)C>[C:1]([NH:5][C:6](=[O:27])[CH2:7][N:8]1[C:14]2[CH:15]=[CH:16][CH:17]=[CH:18][C:13]=2[CH:12]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[CH2:11][CH:10]([N:33]=[N+:34]=[N-:35])[C:9]1=[O:26])([CH3:4])([CH3:3])[CH3:2]参加物
6
反応物 4
生成物 1
試薬・触媒・溶媒 1
反応条件
- 温度
- 75 °C
実験手順
To a 250 ml round-bottomed flask equipped with N2 inlet were added N-tert-butyl-2-[3-bromo-2-oxo-5-phenyl-2,3,4,5-tetrahydro-1H-(1)benzazepin-1-yl] ethanoic acid amide, (8.317 g, 19.37 mmoles), 90 ml dimethylformamide (DMF), and sodium azide (5.25 g, 80 mmoles, under nitrogen), and the mixture was heated at 75° C. for 20 hours with stirring. The reaction mixture was then cooled and distributed between water and ethyl acetate, separated, and the aqueous phase was again extracted. The combined extracts were washed with water three times, with bicarbonate solution once, and then dried with brine and sodium sulfate and filtered and evaporated, leaving a gummy residue, 8.58 g (100%), containing some solvent.
後処理
- customTo a 250 ml round-bottomed flask equipped with N2 inlet
- temperatureThe reaction mixture was then cooled
- customseparated
- extractionthe aqueous phase was again extracted
- washThe combined extracts were washed with water three times, with bicarbonate solution once
- dry with materialdried with brine and sodium sulfate
- filtrationfiltered
- customevaporated
- customleaving a gummy residue, 8.58 g (100%)
- additioncontaining some solvent
出典と根拠
- ORDレコード
- ord-0f850b766acd4aac878515543dd33df7
- 出典データセット
- uspto-grants-1996_01
- 特許番号
- US05484917
関連ノート
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