反応式
Cl[C:2]1[C:11]2[C:6](=[CH:7][C:8]([O:14][CH3:15])=[C:9]([O:12][CH3:13])[CH:10]=2)[N:5]=[CH:4][CH:3]=1.Cl.[Br:17][C:18]1[CH:19]=[CH:20][C:21]2[O:27][CH2:26][CH2:25][NH:24][CH2:23][C:22]=2[CH:28]=1.C(N(C(C)C)CC)(C)C>CN1C(=O)CCC1>[CH3:13][O:12][C:9]1[CH:10]=[C:11]2[C:6](=[CH:7][C:8]=1[O:14][CH3:15])[N:5]=[CH:4][CH:3]=[C:2]2[N:24]1[CH2:23][C:22]2[CH:28]=[C:18]([Br:17])[CH:19]=[CH:20][C:21]=2[O:27][CH2:26][CH2:25]1参加物
5
実験手順
A mixture of commercially available 4-chloro-6,7-dimethoxyquinoline (120 mg, 0.53 mmol), 7-bromo-2,3-dihydro-1,4-benzoxazepine hydrochloride (example 2, step 1) (200 mg, 0.53 mmol), diisopropylethylamine (0.14 g, 1.1 mmol), in NMP (2 mL) was stirred in a microwave reactor at 120° C. for 45 min. After cooling to room temperature, the reaction mixture was purified directly by silica gel flash chromatography (0-10% methanol-dichloromethane gradient) to give 4-[6,7-bis(methyloxy)quinolin-4-yl]-7-bromo-2,3,4,5-tetrahydro-1,4-benzoxazepine (155 mg, 70% yield), MS (EI) for C20H19N2O3: 415 (MH+).
後処理
- customthe reaction mixture was purified directly by silica gel flash chromatography (0-10% methanol-dichloromethane gradient)
出典と根拠
- ORDレコード
- ord-07673876c26f4e7081bfe0b2a7a8501e
- 出典データセット
- uspto-grants-2014_02
- 特許番号
- US08648066B2
関連ノート
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