反応 #1184126

ord-8e9dcc039968418fba609e68a6da4c6f

反応条件

温度
70°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    抽出extracted with ethyl acetate
  2. 2
    洗浄The organic layer was washed with aqueous saturated sodium chloride solution
  3. 3
    乾燥dried with sodium sulfate
  4. 4
    濃縮concentrated under reduced pressure
  5. 5
    その他The residue was purified through silica gel column chromatography

実験手順

A mixture of methyl 4-bromobenzoate (430 mg, 2.00 mmol), 2-benzo[b]thiopheneboronic acid (392 mg, 2.20 mmol), palladium(0) acetate (2.2 mg, 0.010 mmol), potassium carbonate (691 mg, 5.00 mmol), tetrabutylammonium bromide (645 mg, 2.00 mmol) and water (2.2 mL) was stirred in a nitrogen atmosphere at 70° C. for 1 hour. Water was added to the reaction mixture, and extracted with ethyl acetate. The organic layer was washed with aqueous saturated sodium chloride solution, dried with sodium sulfate, and concentrated under reduced pressure. The residue was purified through silica gel column chromatography to obtain the title compound as a pale yellow solid.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08138197B2uspto-grants-2012_03