反応式
Cl[C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[C:9](OC(F)(F)F)[CH:10]=2)[N:5]=[C:4]([N:17]2[CH2:23][C:22]3[CH:24]=[CH:25][CH:26]=[CH:27][C:21]=3[S:20](=[O:29])(=[O:28])[CH2:19][CH2:18]2)[CH:3]=1.[CH3:30][C:31](=[CH2:34])[CH2:32][NH2:33].[CH3:35]N1CCCC1=O>O>[O:28]=[S:20]1(=[O:29])[C:21]2[CH:27]=[CH:26][CH:25]=[CH:24][C:22]=2[CH2:23][N:17]([C:4]2[CH:3]=[C:2]([NH:33][CH2:32][C:31]([CH3:30])=[CH2:34])[C:11]3[C:6](=[CH:7][CH:8]=[C:9]([CH3:35])[CH:10]=3)[N:5]=2)[CH2:18][CH2:19]1参加物
5
反応物 3
生成物 1
試薬・触媒・溶媒 1
反応条件
- 温度
- 160 °C
実験手順
A solution of 4-(4-chloro-6-methylquinolin-2-yl)-2,3,4,5-tetrahydro-1,4-benzothiazepine 1,1-dioxide (372.0 mg, 1.0 mmol, prepared in analogy to 4-(4-chloro-6-(trifluoromethoxy)quinolin-2-yl)-2,3,4,5-tetrahydro-1,4-benzothiazepine 1,1-dioxide in Example 17-1) and 2-methylprop-2-en-1-amine (213.0 mg, 3.0 mmol) in 1-methyl-2-pyrrolidinone (1.0 mL) was heated with stirring at 160° C. for 36 hours. The reaction mixture was cooled to room temperature, diluted with water (10 mL) and extracted with ethyl acetate (100 mL). The organic layer was washed with brine (50 mL×2), dried over anhydrous sodium sulfate and then concentrated in vacuo to afford 407.0 mg of the product as a light yellow solid. MS obsd. (ESI+) [(M+H)+] 408.
後処理
- temperatureThe reaction mixture was cooled to room temperature
- extractionextracted with ethyl acetate (100 mL)
- washThe organic layer was washed with brine (50 mL×2)
- dry with materialdried over anhydrous sodium sulfate
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-2f5d260dc502405c9f7a7cb7335b2994
- 出典データセット
- uspto-grants-2014_10
- 特許番号
- US08871756B2
関連ノート
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