反応式
F[C:2]1[CH:9]=[CH:8][C:5]([C:6]#[N:7])=[CH:4][C:3]=1[C:10]([F:13])([F:12])[F:11].Cl.[CH:15]12[NH:22][CH:19]([CH2:20][CH2:21]1)[CH2:18][CH2:17][CH2:16]2.C(N(CC)C(C)C)(C)C>CS(C)=O>[CH:19]12[N:22]([C:2]3[CH:9]=[CH:8][C:5]([C:6]#[N:7])=[CH:4][C:3]=3[C:10]([F:13])([F:12])[F:11])[CH:15]([CH2:21][CH2:20]1)[CH2:16][CH2:17][CH2:18]2参加物
5
反応条件
- 温度
- 120 °C
実験手順
4-Fluoro-3-(trifluoromethyl)benzonitrile (1.35 g, 7.14 mmol), 8-aza-bicyclo[3.2.1]octane hydrochloride (1.26 g, 8.57 mmol), and N,N-diisopropylethylamine (1.79 g, 13.8 mmol) were combined in DMSO (15 mL) and heated at 120° C. for 24 hours. The mixture was allowed to cool to ambient temperature and partitioned between diethyl ether and saturated NaHCO3 solution. The separated aqueous phase was extracted with diethyl ether and the combined organic layers were washed with water, brine, dried (Na2SO4), filtered, and the filtrate was concentrated under reduced pressure to provide the title compound which was used in the next step without further purification.
後処理
- temperatureto cool to ambient temperature
- custompartitioned between diethyl ether and saturated NaHCO3 solution
- extractionThe separated aqueous phase was extracted with diethyl ether
- washthe combined organic layers were washed with water, brine
- dry with materialdried (Na2SO4)
- filtrationfiltered
- concentrationthe filtrate was concentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-82e318687c99424895ebf2b28a41735b
- 出典データセット
- uspto-grants-2005_08
- 特許番号
- US06933311B2
関連ノート
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