反応 #2050900

ord-e4386e3c611049a8bacb66e8f33863a5

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他Reaction
  2. 2
    ろ過filtered
  3. 3
    その他to remove iron
  4. 4
    その他Reaction
  5. 5
    その他partitioned between ethyl acetate and water
  6. 6
    その他Organic layer separated
  7. 7
    洗浄washed with brine
  8. 8
    乾燥dried over sodium sulfate
  9. 9
    濃縮concentrated

実験手順

4-(2-chloro-5-nitrophenyl)-3-fluoropyridine (1 eq) was stirred with Iron (0), (3 eq), in acetic acid for 10 hours at room temperature. Reaction neutralized with sodium carbonate and filtered to remove iron. Reaction partitioned between ethyl acetate and water. Organic layer separated and washed with brine, dried over sodium sulfate and concentrated to give 4-chloro-3-(3-fluoropyridin-4-yl)benzenamine. HPLC=1.72 min; MS: MH+=223.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08415382B2uspto-grants-2013_04