Реакция #214371

ord-316f168b166d4fa3aaad4f3bb9549663

Уравнение реакции

Nc1cc(Cl)nc(N)n1
6-chloro-2,4-diaminopyrimidine
CNN
methylhydrazine
CN(N)c1cc(N)nc(N)n1
2,4-diamino-6-(1-methylhydrazino)pyrimidine
Выход 56.0%

Реагенты

Нет

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Другоеcould crystallise out
  2. 2
    ФильтрацияThe white solid (3.0 g) was collected by filtration
  3. 3
    Другоеdried under reduced pressure at 70° C
  4. 4
    ДругоеRecrystallisation of the product from methanol/methylhydrazine (50/l)

Методика

To a refluxing solution of 6-chloro-2,4-diaminopyrimidine (4.0 g) in anhydrous methanol (40 ml) was added methylhydrazine (3.2 g). After 18 hours the refluxing mixture was allowed to cool to room temperature under a nitrogen atmosphere in order that the product could crystallise out. The white solid (3.0 g) was collected by filtration and dried under reduced pressure at 70° C. Recrystallisation of the product from methanol/methylhydrazine (50/l) gave straw-coloured crystals of 2,4-diamino-6-(1-methylhydrazino)pyrimidine (1.92 g; 56% of theoretical yield; M.P. 214°-217° C. decomposition).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US04255427uspto-grants-1981_03