Trifluoroacetic acid → HCID 23149183、化合物
反応式
[Cl:1][C:2]([Cl:19])([F:18])[S:3][C:4]1[CH:5]=[N:6][N:7](CC2C=CC(OC)=CC=2)[CH:8]=1.FC(F)(F)C(O)=O.C(=O)([O-])O.[Na+]>>[Cl:1][C:2]([Cl:19])([F:18])[S:3][C:4]1[CH:5]=[N:6][NH:7][CH:8]=1参加物
4
反応条件
- 温度
- 65 °C
実験手順
1.04 g of 4-{[dichlorofluoromethyl]thio}-1-(4-methoxybenzyl)-1H-pyrazole was dissolved to 6 ml of trifluoroacetic acid, followed by stirring at 65° C. for 3 hours. After the reaction mixture was cooled to room temperature, it was added to saturated aqueous solution of sodium hydrogen carbonate. The mixture was extracted with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate, and filtered. The filtrate was concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to obtain 0.19 g of 4-{[dichlorofluoromethyl]thio}-1H-pyrazole.
後処理
- temperatureAfter the reaction mixture was cooled to room temperature
- extractionThe mixture was extracted with ethyl acetate
- dry with materialThe organic layer was dried over anhydrous sodium sulfate
- filtrationfiltered
- concentrationThe filtrate was concentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-131e44626a8d4a1390e459e58d5a8591
- 出典データセット
- uspto-grants-2009_06
- 特許番号
- US07541374B2
反応ノート
読み込み中…