反応 #218772

ord-c5c0153794f24a8f9f283fc164916f4b

反応条件

温度
130°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    抽出extracted with ethyl acetate (2×25 ml)
  2. 2
    洗浄The combined organic layer was washed with 5% hydrochloric acid
  3. 3
    乾燥dried over anhydrous sodium sulfate

実験手順

Intermediate 2-bromo-4-cyclopentoxy-3-(p-nitrophenoxy)-benzaldehyde (500 mg, 1.09 mmol), anhydrous sodium carbonate (150 mg, 1.325 mmol) and palladium (II) acetate (25 mg, 0.096 mmol), in dimethylformamide (10 ml) are heated and stirred under nitrogen at 130° C. for 7 h. Water (90 ml) is added to the cooled reaction mixture and extracted with ethyl acetate (2×25 ml). The combined organic layer was washed with 5% hydrochloric acid followed by water and dried over anhydrous sodium sulfate to afford the product as a yellow solid (200 mg). mp: 230-240° C.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07384962B2uspto-grants-2008_06