反応 #92113
ord-e7bd272bccab47cd996ea45e00d8bdd3
反応条件
温度
80°CELSIUS
詳細条件
See reaction.notes.procedure_details.
後処理
- 1その他Into a 250-mL round-bottom flask, was placed
- 2濃縮The resulting mixture was concentrated under vacuum
- 3workup.ADDITIONThe resulting solution was diluted with 200 mL of H2O
- 4抽出The resulting solution was extracted with 4×100 mL of ethyl acetate
- 5洗浄The resulting mixture was washed with 2×100 mL of brine
- 6乾燥The mixture was dried over anhydrous sodium sulfate
- 7その他This resulted in 5 g (90%) of (3-chloropropyl)(2,2,2-trifluoroethyl)amine as a light yellow liquid
実験手順
Into a 250-mL round-bottom flask, was placed N-(3-chloropropyl)-2,2,2-trifluoroacetamide (6 g, 31.65 mmol, 1.00 equiv), tetrahydrofuran (30 mL), BH3/THF (80 mL). The resulting solution was stirred for 3 h at 80° C. in an oil bath. The resulting mixture was concentrated under vacuum. The resulting solution was diluted with 200 mL of H2O. The resulting solution was extracted with 4×100 mL of ethyl acetate and the organic layers combined. The resulting mixture was washed with 2×100 mL of brine. The mixture was dried over anhydrous sodium sulfate. This resulted in 5 g (90%) of (3-chloropropyl)(2,2,2-trifluoroethyl)amine as a light yellow liquid.