반응 #660234

ord-034151b1331a4c608ec883ea14fc4e6a

반응 조건

온도
50°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타the layers were separated
  2. 2
    추출The aqueous layer was extracted with ethyl acetate
  3. 3
    건조the combined organic layers were dried over MgSO4
  4. 4
    여과filtered
  5. 5
    농축concentrated
  6. 6
    기타The residue was purified by flash chromatography (5% 7N NH3 in methanol-dichloromethane)

실험 절차

A solution of 3-(benzyloxy)phenol (2.002 g), 2-chloro-N,N-dimethylethanamine (1.459 g) in N,N-dimethylformamide (50 mL) was treated with cesium carbonate (3.91 g) and stirred at 50° C. overnight. The mixture was diluted with ethyl acetate and 1N aqueous NaOH and the layers were separated. The aqueous layer was extracted with ethyl acetate and the combined organic layers were dried over MgSO4, filtered and concentrated. The residue was purified by flash chromatography (5% 7N NH3 in methanol-dichloromethane) to give the desired product.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09029404B2uspto-grants-2015_05