반응 #96175

ord-6a0e11892b014bdcbc21695dc4dabf20

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    여과The DCC-urea was filtered
  2. 2
    세척washed with CH2Cl2
  3. 3
    세척The filtrate was then washed 2×125 ml 1N HCl, 2×125 ml saturated NaHCO3, 2×125 ml brine
  4. 4
    건조dried (MgSO4)
  5. 5
    여과filtered
  6. 6
    농축concentrated

실험 절차

2-Acetylthio-3-chlorobenzoic acid (11.5 g, 50 mmol) and N-cyclopentylglycine t-butyl ester (10.0 g, 50 mmol) in methylene chloride (350 ml) were cooled to 0°-5° C., and N,N1 -dicyclohexylcarbodiimide (10.3 g, 50 mmol) in methylene chloride (50 ml) was added. The mixture was stirred overnight. The DCC-urea was filtered and washed with CH2Cl2. The filtrate was then washed 2×125 ml 1N HCl, 2×125 ml saturated NaHCO3, 2×125 ml brine, dried (MgSO4), filtered and concentrated to give 20.6 g of an oil. The crude product was used without further purification in the next step.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04347246uspto-grants-1982_08