反応式
[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[O:11][CH2:10][CH2:9][N:8]([C:12](Cl)=[O:13])[CH2:7][C:6]=2[CH:15]=1.[F:16][C:17]([F:32])([F:31])[C:18]1[CH:19]=[C:20]([C:24]2([OH:30])[CH2:29][CH2:28][NH:27][CH2:26][CH2:25]2)[CH:21]=[CH:22][CH:23]=1.C(N(C(C)C)CC)(C)C>ClCCl.C(OCC)(=O)C>[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[O:11][CH2:10][CH2:9][N:8]([C:12]([N:27]3[CH2:26][CH2:25][C:24]([C:20]4[CH:21]=[CH:22][CH:23]=[C:18]([C:17]([F:16])([F:31])[F:32])[CH:19]=4)([OH:30])[CH2:29][CH2:28]3)=[O:13])[CH2:7][C:6]=2[CH:15]=1参加物
6
反応物 3
生成物 1
試薬・触媒・溶媒 2
実験手順
A solution of 7-bromo-2,3-dihydro-1,4-benzoxazepine-4(5H)-carbonyl chloride (example 2) (0.400 g, 1.38 mmol), 4-(3-(trifluoromethyl)phenyl)piperidin-4-ol (0.371 g, 1.51 mmol), and diisopropylethylamine (0.535 g, 4.14 mmol) in dichloromethane (3 mL) was stirred at room temperature for 1 hour. The reaction mixture was diluted with ethyl acetate (50 mL), washed with 10% citric acid (20 mL) and brine (20 mL). The organic layer was dried over sodium sulfate. Filtration and concentration afforded 1-[(7-bromo-2,3-dihydro-1,4-benzoxazepin-4(5H)-yl)carbonyl]-4-[3-(trifluoromethyl)phenyl]piperidin-4-ol (0.688 g, 100%) as a white solid that was used without further purification. MS (EI) for C22H22BrF3N2O3: 500 (MH+).
後処理
- washwashed with 10% citric acid (20 mL) and brine (20 mL)
- dry with materialThe organic layer was dried over sodium sulfate
- filtrationFiltration and concentration
出典と根拠
- ORDレコード
- ord-3e1f61430f1a49f780df481a54dbea9d
- 出典データセット
- uspto-grants-2014_01
- 特許番号
- US08637499B2
関連ノート
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