反応式
[Cl:1][C:2]1[CH:15]=[C:14]([Cl:16])[CH:13]=[CH:12][C:3]=1[O:4][C:5]1[CH:11]=[CH:10][C:8]([NH2:9])=[CH:7][CH:6]=1.C[N:18]([CH:20]=O)C.Br[CH2:23][C:24]([C:26]1[CH:31]=[CH:30][C:29]([O:32][CH2:33][CH2:34][CH2:35][N:36]([CH2:39][CH3:40])[CH2:37][CH3:38])=[CH:28][CH:27]=1)=O>O.CCOC(C)=O>[CH2:15]([C:20]1[N:9]([C:8]2[CH:7]=[CH:6][C:5]([O:4][C:3]3[CH:12]=[CH:13][C:14]([Cl:16])=[CH:15][C:2]=3[Cl:1])=[CH:11][CH:10]=2)[CH:23]=[C:24]([C:26]2[CH:31]=[CH:30][C:29]([O:32][CH2:33][CH2:34][CH2:35][N:36]([CH2:39][CH3:40])[CH2:37][CH3:38])=[CH:28][CH:27]=2)[N:18]=1)[CH2:2][CH2:3][CH3:12]参加物
反応物 3
生成物 1
試薬・触媒・溶媒 2
実験手順
To a stirred solution of 4-(2,4-dichloro-phenoxy)aniline described above (1.2 eq., 5.2 mmol) in anhydrous DMF (20 mL) DIEA (3 eq. 15 mmol) was added, followed by slow addition of the 2-bromo-1-{4-[3-(diethylamino)propoxy]phenyl}ethanone described above (4.4 mmol), according to General Procedure R2. The reaction mixture was stirred under nitrogen at rt until completion, as indicated by TLC or HPLC. The reaction mixture was then diluted with cold H2O and the product was isolated in EtOAc. The combined organic layers were washed with brine and dried over sodium sulfate. Evaporation of solvent in vacuuo afforded the desired product. The crude alkylated aniline was purified by chromatography (Silica gel). Pure product obtained from 2-4% MeOH/DCM (yield˜5%).
後処理
- additionwas added
- washThe combined organic layers were washed with brine
- dry with materialdried over sodium sulfate
- customEvaporation of solvent in vacuuo
出典と根拠
- ORDレコード
- ord-87a8c2665d60444d8cefb43d28d919e3
- 出典データセット
- uspto-grants-2010_06
- 特許番号
- US07737285B2
関連ノート
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