反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:9]([C:13]([O:15][CH2:16][CH3:17])=[O:14])=[CH:10][NH:11][CH:12]=2)=[CH:4][CH:3]=1.[F:18][C:19]([F:23])([F:22])[S:20]Cl>C(Cl)Cl>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[C:9]([C:13]([O:15][CH2:16][CH3:17])=[O:14])=[CH:10][NH:11][C:12]=2[S:20][C:19]([F:23])([F:22])[F:18])=[CH:4][CH:3]=1参加物
反応条件
- 温度
- -30 °C
実験手順
A solution of ethyl 4-(p-chlorophenyl)-pyrrole-3-carboxylate (9.0 g, 0,036 mol) in methylene chloride (180 mL) is treated with trifluoromethylsulfenyl chloride (4.9 g, 0.036 mol) with stirring for 45 minutes at -30° C. The reaction mixture is warmed to room temperature and stirred for several hours. Since a TLC shows some starting material present, the reaction mixture is cooled to -30° C., treated with additional trifluoromethylsulfenyl chloride (1.3 g, 0.0095 mol), warmed to room temperature overnight with stirring, washed with water, saturated sodium hydrogen carbonate solution and brine, dried over anhydrous magnesium sulfate and concentrated in vacuo to give the title product as an off-white solid (12.0 g, mp 161.5°-164.0° C.) which is identified by 1HNMR, 19FNMR and 13CNMR spectral analyses.
後処理
- temperatureThe reaction mixture is warmed to room temperature
- stirringstirred for several hours
- temperaturethe reaction mixture is cooled to -30° C.
- temperaturewarmed to room temperature overnight
- stirringwith stirring
- washwashed with water, saturated sodium hydrogen carbonate solution and brine
- dry with materialdried over anhydrous magnesium sulfate
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-e21a252a88244b3a9d0b69f9180d2ee6
- 出典データセット
- uspto-grants-1996_01
- 特許番号
- US05484807
関連ノート
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