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. 1
    その他Into a 250-mL round-bottom flask, was placed
  2. 2
    濃縮The resulting mixture was concentrated under vacuum
  3. 3
    workup.ADDITIONThe resulting solution was diluted with 200 mL of H2O
  4. 4
    抽出The resulting solution was extracted with 4×100 mL of ethyl acetate
  5. 5
    洗浄The resulting mixture was washed with 2×100 mL of brine
  6. 6
    乾燥The mixture was dried over anhydrous sodium sulfate
  7. 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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US09447084B2uspto-grants-2016_09