반응 #3190

ord-83eb8c4f8a924307bcc393ec98b1dc0e

용매

반응 조건

온도
60°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.WAITplaced in the freezer for several hours
  2. 2
    여과The product was then collected by filtration
  3. 3
    세척washed with a small amount of cold ethanol
  4. 4
    기타recrystallized from dichloromethane-ethanol

실험 절차

3,4-Diethylpyrrole (2A, FIG. 2)28 (0.6, 4.9 mmol), benzyl 5-(acetoxymethyl)-3-methyl-4-ethyl-pyrrole-2-carboxylate (2B, FIG. 2)29 (2.5 g, 7.9 mmol), and p-toluenesulfonic acid (0.15 g) were dissolved in 60 mL of absolute ethanol and heated at 60° C. for 8 h under nitrogen. The resulting suspension was reduced in volume to 30 mL and placed in the freezer for several hours. The product was then collected by filtration, washed with a small amount of cold ethanol, and recrystallized from dichloromethane-ethanol to afford a white powder (2.07 g, 82%): mp 211° C. NMR spectra and high resolution mass spectral data were obtained as described and are reported 13a.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05733903uspto-grants-1998_03