反応式
[H-].[Na+].ClC1C2N=C(CC(F)(F)F)[N:9](Cl)C=2C=CC=1.[Cl:19][C:20]1[CH:21]=[C:22]2[C:26](=[CH:27][C:28]=1[Cl:29])[NH:25][C:24]([CH2:30][C:31]([F:34])([F:33])[F:32])=C2.Br[CH2:36][C:37]([C:39]1[C:40]([C:45]2[CH:50]=[CH:49][CH:48]=[CH:47][CH:46]=2)=[N:41][O:42][C:43]=1[CH3:44])=[O:38].[NH4+].[Cl-]>CN(C=O)C>[Cl:29][C:28]1[C:20]([Cl:19])=[CH:21][C:22]2[N:9]([CH2:36][C:37]([C:39]3[C:40]([C:45]4[CH:50]=[CH:49][CH:48]=[CH:47][CH:46]=4)=[N:41][O:42][C:43]=3[CH3:44])=[O:38])[C:24]([CH2:30][C:31]([F:32])([F:33])[F:34])=[N:25][C:26]=2[CH:27]=1参加物
反応物 5
生成物 1
試薬・触媒・溶媒 1
反応条件
- 温度
- 0 °C
実験手順
NaH (60%) (60 mg, 1.5 mmol) was added into a solution of dichloro-2-(2,2,2-trifluoro-ethyl)-1H-benzoimidazole. 5,6-Dichloro-2-(2,2,2-trifluoro-ethyl)-1H-indole (269 mg, 1 mmol) in DMF (5 ml) at 0° C. The resulting mixture was stirred at 0° C. for half hours. 2-bromo-1-(5-methyl-3-phenylisoxazol-4-yl)ethan-1-one (420 mg, 1.5 mmol) was then added to the reaction mixture at 0° C. The reaction temperature was raised to 25° C. and then the reaction mixture was stirred for 18 hours. NH4Cl (aq.) was added and extracted with EtOAc. The organic layer was washed with brine, then dried over anhydrous MgSO4. The solvent was distilled out under reduced pressure. Column chromatography (silica gel, EtOAc/hexanes (0% to 60%) yielded the title compound as a white solid.
後処理
- customat 0° C
- temperatureThe reaction temperature was raised to 25° C.
- stirringthe reaction mixture was stirred for 18 hours
- extractionextracted with EtOAc
- washThe organic layer was washed with brine
- dry with materialdried over anhydrous MgSO4
- distillationThe solvent was distilled out under reduced pressure
出典と根拠
- ORDレコード
- ord-ffff62f7bc4a4bfda5129fdd0db1be83
- 出典データセット
- uspto-grants-2009_07
- 特許番号
- US07566733B2
関連ノート
読み込み中…