反応式
[C:1]([NH:4][C:5]1[N:10]=[CH:9][C:8]([NH:11][C:12](=[O:19])OCC(Cl)(Cl)Cl)=[CH:7][CH:6]=1)(=[O:3])[CH3:2].[F:20][C:21]1[C:26]([F:27])=[CH:25][CH:24]=[CH:23][C:22]=1[C:28]1[N:29]=[C:30]([N:33]2[CH2:38][CH2:37][NH:36][CH2:35][CH2:34]2)[S:31][CH:32]=1.C(N(C(C)C)CC)(C)C.O>CS(C)=O>[C:1]([NH:4][C:5]1[N:10]=[CH:9][C:8]([NH:11][C:12]([N:36]2[CH2:37][CH2:38][N:33]([C:30]3[S:31][CH:32]=[C:28]([C:22]4[CH:23]=[CH:24][CH:25]=[C:26]([F:27])[C:21]=4[F:20])[N:29]=3)[CH2:34][CH2:35]2)=[O:19])=[CH:7][CH:6]=1)(=[O:3])[CH3:2]参加物
6
反応物 4
生成物 1
試薬・触媒・溶媒 1
反応条件
- 温度
- 70 °C
実験手順
A mixture of 2,2,2-trichloroethyl [6-(acetylamino)pyridin-3-yl]carbamate (255 mg, 0.782 mmol), 1-[4-(2,3-difluorophenyl)-1,3-thiazol-2-yl]piperazine (200 mg, 0.711 mmol) and diisopropylethylamine (0.248 ml, 1.42 mmol) in dimethyl sulfoxide (2.5 ml) was stirred at 70° C. for 15 hours. Water was poured to the reaction mixture, and the mixture was extracted with ethyl acetate. The extract was washed with water, and dried over magnesium sulfate anhydrous, and the solvent was distilled off under reduced pressure. The residue was recrystallized from a mixed solvent of hexane and tetrahydrofuran to give 119 mg (36.6%) of the desired product as a solid.
後処理
- extractionthe mixture was extracted with ethyl acetate
- washThe extract was washed with water
- dry with materialdried over magnesium sulfate anhydrous
- distillationthe solvent was distilled off under reduced pressure
- customThe residue was recrystallized from a mixed solvent of hexane and tetrahydrofuran
出典と根拠
- ORDレコード
- ord-953e60912b1a4915ae3b8791bd2eb1c3
- 出典データセット
- uspto-grants-2010_12
- 特許番号
- US07851473B2
関連ノート
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