반응 #3367

ord-612c475449ba4056a49ab5f66bcc7953

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The mixture was heated
  2. 2
    온도at reflux for 2 hours
  3. 3
    온도cooled
  4. 4
    농축concentrated to an oil
  5. 5
    기타the solid was collected
  6. 6
    기타recrystallized in ethanol

실험 절차

To 4.1 g (0.012 mol) of 8-mercapto-[1,3]dioxolo [4,5-g]quinoline-7-carboxylic acid (2-pyridin-2-yl-ethyl)-amide (from Preparation 34) and 5 mL (0.035 mol) of triethylamine in 750 mL of methanol was added 2.95 g (0.012 mol) of iodine in 100 mL of methanol. The mixture was heated at reflux for 2 hours, cooled, and then concentrated to an oil. The residue was slurried in water, and the solid was collected and recrystallized in ethanol to give 3.5 g of the title compound, mp 200°-201° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05733921uspto-grants-1998_03