Реакция #4390

ord-9d28aa19805e4a3182693ceb169ad3c2

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Температураwas refluxed for 24 hours under a nitrogen atmosphere
  2. 2
    Другоеto stand at room temperature
  3. 3
    Экстракцияextracted with ethyl acetate
  4. 4
    ПромывкаThe extract was washed with water
  5. 5
    Сушкаdried over magnesium sulfate
  6. 6
    Другоеevaporated in vacuo
  7. 7
    ДругоеThe residue was purified by column chromatography on silica gel (110 g) with a mixture of chloroform and methanol (100:3) as an eluent

Методика

A mixture of 2-amino-3-chloropyrazine (4.3 g), 2-methylbenzylamine (4.6 g), potassium carbonate (5.5 g), and potassium iodide (0.4 g) in N,N-dimethylformamide (43 ml) was refluxed for 24 hours under a nitrogen atmosphere and allowed to stand at room temperature. The mixture was poured into water and extracted with ethyl acetate. The extract was washed with water, dried over magnesium sulfate, and evaporated in vacuo. The residue was purified by column chromatography on silica gel (110 g) with a mixture of chloroform and methanol (100:3) as an eluent to give 2-amino-3-(2-methylbenzylamino)pyrazine (1.4 g).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US04725601uspto-grants-1988_02