반응 #164108

ord-16b2910dc5ad4b0c922ddeaeaa3e2eeb

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도with reflux
  2. 2
    온도the mixture was cooled
  3. 3
    세척washed with NaHCO3 solution and saturated NaCl solution
  4. 4
    건조dried with Na2SO4
  5. 5
    농축concentrated to low volume in a vacuum

실험 절차

The title compound of step 2 (43.3 g, 217 mmol) and ethylene glycol (27.4 g, 435 mmol) were boiled in toluol (430 mL) with the addition of p-toluol sulphonic acid (1.87 g, 10.9 mmol) at a water separator for 3 h with reflux. After the reaction had ended, the mixture was cooled, washed with NaHCO3 solution and saturated NaCl solution, dried with Na2SO4 and concentrated to low volume in a vacuum.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08835689B2uspto-grants-2014_09