反応 #47085

ord-97b8abf3cd92466dbc6e97fe3e267b20

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    洗浄the mixture is washed with water, brine
  2. 2
    乾燥dried (MgSO4)
  3. 3
    ろ過filtered
  4. 4
    その他The filtrate is evaporated
  5. 5
    workup.DISTILLATIONdistilled (130-140° C.)

実験手順

To a solution of thiophenol (1 mL, 9.7 mmol) in DMF (20 mL) is added potassium carbonate (1.51 g, 10.9 mmol) and ethyl bromoacetate (1.17 mL, 10.6 mmol), and the mixture is stirred at RT for 25 min. Et2O is added, and the mixture is washed with water, brine, then dried (MgSO4), and filtered. The filtrate is evaporated, and the residue is vacuum distilled (130-140° C.) to give 1.71 g of the product 400. 1H NMR (CDCl3) δ 7.41 (d, 2H), 7.33-7.2 (m, 4H), 4.16 (q, 2H), 3.63 (s, 2H), 1.22 (t, 3H); MS: m/z 196 (M++1).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07741493B2uspto-grants-2010_06