反応式
ClC(Cl)(Cl)CO[C:5](=[O:17])[NH:6][C:7]1[CH:8]=N[C:10]([NH:13][C:14](=[O:16])[CH3:15])=[CH:11][CH:12]=1.[S:20]1[CH:24]=[CH:23][C:22]([C:25]2[CH:26]=[C:27]([N:31]3[CH2:36][CH2:35][NH:34][CH2:33][CH2:32]3)[CH:28]=[CH:29][CH:30]=2)=[CH:21]1.[CH:37](N(C(C)C)CC)(C)C.O>CS(C)=O>[C:14]([NH:13][C:10]1[CH:11]=[CH:12][C:7]([NH:6][C:5]([N:34]2[CH2:35][CH2:36][N:31]([C:27]3[CH:28]=[CH:29][CH:30]=[C:25]([C:22]4[CH:23]=[CH:24][S:20][CH:21]=4)[CH:26]=3)[CH2:32][CH2:33]2)=[O:17])=[CH:8][CH:37]=1)(=[O:16])[CH3:15]参加物
6
反応物 4
生成物 1
試薬・触媒・溶媒 1
実験手順
A mixed solution of 2,2,2-trichloroethyl[6-(acetylamino)pyridin-3-yl]carbamate (147 mg, 0.450 mmol), 1-[3-(3-thienyl)phenyl]piperazine (100 mg, 0.409 mmol) and diisopropylethylamine (0.143 ml, 0.818 mmol) in dimethylsulfoxide (1.5 ml) was stirred at 70° C. for 15 hours. Water was poured into the reaction solution, and extracted with ethyl acetate. The extract was washed with water, dried over anhydrous magnesium sulfate, and the solvent was distilled away under reduce pressure. The residue was purified by silica gel column chromatography (ethyl acetate), and recrystallized from a mixed solvent of hexane and tetrahydrofuran to give the titled compound 85.5 mg (51.5%) as solid product.
後処理
- extractionextracted with ethyl acetate
- washThe extract was washed with water
- dry with materialdried over anhydrous magnesium sulfate
- distillationthe solvent was distilled away
- customThe residue was purified by silica gel column chromatography (ethyl acetate)
- customrecrystallized from a mixed solvent of hexane and tetrahydrofuran
出典と根拠
- ORDレコード
- ord-a3b717ebb86741f5af12ade3a8fca844
- 出典データセット
- uspto-grants-2010_10
- 特許番号
- US07812025B2
関連ノート
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