反応 #1107086

ord-8d50fac1fdcc4edf8534c807ab7df098

反応条件

温度
78°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他Then potassium carbonate is removed by filtration
  2. 2
    濃縮the mother liquid is concentrated
  3. 3
    その他to give a crude that
  4. 4
    その他is purified by column chromatography (silica gel, eluent: cyclohexane 100%)

実験手順

Potassium carbonate (2.50 g, 18.07 mmol, 2.1 eq) is added at room temperature to a stirred solution of thiophene-2-thiol (813 μL, 8.61 mmol, 1.0 eq) in 1,2-dibromoethane (10 mL) and the resulting mixture is stirred at 78° C. for 3 hours. Then potassium carbonate is removed by filtration and the mother liquid is concentrated to give a crude that is purified by column chromatography (silica gel, eluent: cyclohexane 100%) to afford 2-(2-bromo-ethylsulfanyl)-thiophene as a light yellow oil (1.86 g, 95% yield).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08716280B2uspto-grants-2014_05