反応 #628751

ord-4f0c3899bd84488e92ef2913d9370889

反応条件

温度
100°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度The mixture was cooled to rt
  2. 2
    抽出extracted with ethyl acetate
  3. 3
    洗浄The extracts were washed with brine
  4. 4
    乾燥dried over sodium sulfate
  5. 5
    その他evaporated

実験手順

4-Bromo-1-fluoro-2-nitrobenzene (1.0 g, 4.5 mmol) [Aldrich] and potassium carbonate (1.6 g, 11 mmol) were stirred in N,N-dimethylformamide (10 mL), and 2-propanethiol (0.42 mL, 4.5 mmol) was added. The mixture was heated to 100° C. for 16 hours. The mixture was cooled to rt, diluted with water (100 mL), and extracted with ethyl acetate. The extracts were washed with brine, dried over sodium sulfate, and evaporated to give the desired compound (1.2 g, 96%). 1H NMR (300 MHz, CDCl3): δ 8.27 (s, 1H), 7.62 (d, 1H), 7.38 (d, 1H), 3.55 (m, 1H), 1.40 (d, 6H).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08871753B2uspto-grants-2014_10