반응 #359103

ord-52e9f44e93424b29b858672ddf591cb9

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    추출the mixture was extracted with dichloromethane (3×)
  2. 2
    세척The combined organic extracts were washed with saturated brine
  3. 3
    건조dried over magnesium sulfate
  4. 4
    여과filtered
  5. 5
    농축concentrated
  6. 6
    기타Purification by silica gel chromatography [100% dichloromethane→95% dichloromethane/5% (10% ammonium hydroxide/methanol)]

실험 절차

Triethylamine (16.0 mL, 114 mmol) was added to a solution of 2,4-dimethoxybenzylamine hydrochloride (11.1 g, 54.5 mmol) and 2,3-dibromopropene (10.9 g, 54.5 mmol) in dichloromethane (200 mL). After 18 h, water was added and the mixture was extracted with dichloromethane (3×). The combined organic extracts were washed with saturated brine, dried over magnesium sulfate, filtered and concentrated. Purification by silica gel chromatography [100% dichloromethane→95% dichloromethane/5% (10% ammonium hydroxide/methanol)] gave the title compound (7.85 g).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07452903B2uspto-grants-2008_11