반응 #71872

ord-44b331cbf319449888b2dd62743014fb

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    세척The reaction solution was washed with water and brine
  2. 2
    건조dried over anhydrous magnesium sulfate
  3. 3
    농축concentrated under reduced pressure
  4. 4
    기타The residue was purified by silica gel column chromatography (elution solvent: ethyl acetate/hexane=1/2, 1/1, 2/1, 1/0)

실험 절차

Dichloromethane (80 mL) was added to serine methyl ester hydrochloride (2.64 g, 17 mmol), 3-methoxy-4-nitrobenzoic acid (3 g, 15.2 mmol), WSC hydrochloride (3.83 g, 20 mmol), DMAP (0.18 g, 1.5 mmol) and N,N-diisopropylethylamine (2.58 g, 20 mmol), and the mixture was stirred at room temperature for one day. The reaction solution was washed with water and brine, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (elution solvent: ethyl acetate/hexane=1/2, 1/1, 2/1, 1/0) to obtain 3.11 g of the title compound as a colorless solid (69%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08536197B2uspto-grants-2013_09