Реакция #75114

Уравнение реакции

2,4-diamino-6-[3,6-dihydro-1(2H)-pyridyl]pyrimidine-3-oxide

methylene chloride

chloroformic acid butyl ester

→

dibutyl 6-[3,6-dihydro-1(2H)-pyridyl]-2,4-pyrimidine-dicarbamate-3-oxide

Растворители

triethylamine

Условия реакции

Обработка

1. 1
   workup.ADDITIONThe mixture is treated with 45 ml
2. 2
   ДругоеThe mixture obtained
3. 3
   Промывкаis washed with water
4. 4
   Экстракцияextracted with methylene chloride
5. 5
   Другоеevaporated under reduced pressure
6. 6
   ДругоеThe residue is recrystallized from ethanol, there

Методика

20 G. of 2,4-diamino-6-[3,6-dihydro-1(2H)-pyridyl]pyrimidine-3-oxide are mixed with 250 ml. of methylene chloride and 35 ml. of triethylamine, stirred and cooled to 5° C. The mixture is treated with 45 ml. of chloroformic acid butyl ester and stirred at room temperature for 6 hours. The mixture obtained is washed with water, extracted with methylene chloride and evaporated under reduced pressure. The residue is recrystallized from ethanol, there being obtained dibutyl 6-[3,6-dihydro-1(2H)-pyridyl]-2,4-pyrimidine-dicarbamate-3-oxide, having a melting point of 131°-132° C.

Источник