반응 #47085

ord-97b8abf3cd92466dbc6e97fe3e267b20

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    세척the mixture is washed with water, brine
  2. 2
    건조dried (MgSO4)
  3. 3
    여과filtered
  4. 4
    기타The filtrate is evaporated
  5. 5
    workup.DISTILLATIONdistilled (130-140° C.)

실험 절차

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).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07741493B2uspto-grants-2010_06