Реакция #55502

ord-0cbe754051c04555a9debb952b65163a

Уравнение реакции

CCO
ethanol
Nc1cc(Cl)nc(N)n1
2,4-diamino-6-chloropyrimidine
CCO
ethanol
[Na+].[OH-]
sodium hydroxide
O=C(OO)c1cccc(Cl)c1
3-chloro-perbenzoic acid
Nc1cc(Cl)nc(N)[n+]1[O-]
2,4-diamino-6-chloropyrimidine-3-oxide

Растворители

Условия реакции

Температура
-10°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Другоеat 35° C
  2. 2
    workup.WAITleft
  3. 3
    workup.WAITto stand at 5° C. overnight
  4. 4
    ФильтрацияThe solid material is filtered off
  5. 5
    Другоеrecrystallized from ethanol, there

Методика

75 g. of 2,4-diamino-6-chloropyrimidine are dissolved in 1500 ml. of ethanol at 35° C. The solution is cooled to -10° C. and a solution of 100 g. of 3-chloro-perbenzoic acid in 500 ml. of ethanol is slowly added dropwise in the course of 1 hour. The suspension is subsequently stirred at -10° C. for 7 hours and left to stand at 5° C. overnight. The suspension is neutralized with 24 g. of sodium hydroxide in 100 ml. of water. The solid material is filtered off and recrystallized from ethanol, there being obtained pure 2,4-diamino-6-chloropyrimidine-3-oxide.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US04220772uspto-grants-1980_09