반응 #48730

ord-37767759e28946f6af4b9007458d87cf

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도Warm
  2. 2
    기타reaction mixture to 12° C. over 3.5 hours
  3. 3
    세척wash with 5% aqueous citric acid (3×20 mL)
  4. 4
    건조Dry over magnesium sulfate
  5. 5
    농축concentrate under reduced pressure

실험 절차

Cool a solution of (+/−)-trans-2-hydroxymethyl-cyclopropanecarboxylic acid ethyl ester (0.22 g, 1.53 mmol) in 1.5 mL DMSO to 0° C. Add to the frozen solution triethyl-amine (0.85 mL, 0.62 mmol) followed by sulfur trioxide pyridine (0.49 g, 3.05 mmol). Warm reaction mixture to 12° C. over 3.5 hours, dilute with diethyl ether (80 mL), and wash with 5% aqueous citric acid (3×20 mL) followed by saturated aqueous sodium chloride (1×20 mL). Dry over magnesium sulfate and concentrate under reduced pressure to provide the desired compound.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07745438B2uspto-grants-2010_06