Реакция #55502
ord-0cbe754051c04555a9debb952b65163a
Уравнение реакции
ethanol
2,4-diamino-6-chloropyrimidine
ethanol
sodium hydroxide
3-chloro-perbenzoic acid
→
2,4-diamino-6-chloropyrimidine-3-oxide
Реагенты
Нет
Растворители
Условия реакции
Температура
-10°CELSIUS
Подробные условия
See reaction.notes.procedure_details.
Обработка
- 1Другоеat 35° C
- 2workup.WAITleft
- 3workup.WAITto stand at 5° C. overnight
- 4ФильтрацияThe solid material is filtered off
- 5Другоеrecrystallized 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.