تفاعل #3367

ord-612c475449ba4056a49ab5f66bcc7953

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةThe mixture was heated
  2. 2
    درجة الحرارةat reflux for 2 hours
  3. 3
    درجة الحرارةcooled
  4. 4
    تركيزconcentrated to an oil
  5. 5
    أخرىthe solid was collected
  6. 6
    أخرىrecrystallized in ethanol

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05733921uspto-grants-1998_03