Реакция #5831

ord-d4ee0e39c1e94258bf77463d69e44f83

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Экстракцияextracted twice with 200 ml of chloroform
  2. 2
    СушкаThe extract was dried over magnesium sulfate
  3. 3
    Концентрированиеconcentrated under a reduced pressure
  4. 4
    Другоеresulting residue
  5. 5
    Промывкаeluted with chloroform/methanol (100:1 to 50:1)

Методика

7.71 g of p-chlorocinnamyl chloride and 13.5 g of 2,3-diaminopyridine were dissolved in 220 ml of dimethylformamide, and to the solution was added 8.6 g of potassium carbonate, and the mixture was stirred at a room temperature for 50 hours, and after adding 300 ml of water, extracted twice with 200 ml of chloroform. The extract was dried over magnesium sulfate and concentrated under a reduced pressure, and resulting residue was applied to a silica gel column and eluted with chloroform/methanol (100:1 to 50:1), to obtain 4.52 g of the title compound as yellow crystals.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US05245034uspto-grants-1993_09