Реакция #70245

Уравнение реакции

4-chloro-2-methylsulfanyl-pyrimidine

hydrazine

potassium carbonate

→

N-(2-methylsulfanyl-pyrimidin-4-yl)-hydrazine

Выход 57.6%

Растворители

ethanol

Условия реакции

Обработка

1. 1
   ТемператураThe mixture was refluxed for 3 hrs
2. 2
   Фильтрацияfiltered
3. 3
   ПромывкаThe filtered solid was rinsed with ethanol (30 mL)
4. 4
   ДругоеThe combined ethanol solution was evaporated
5. 5
   Другоеto give a crude oily mixture which
6. 6
   Другоеwas purified by ISCO flash column chromatography (30% to 100% ethyl acetate in hexanes)

Методика

In a 250 mL round bottom flask, 4-chloro-2-methylsulfanyl-pyrimidine (5 g, 31.1 mmol), hydrazine (4.5 g, 140 mmol) and potassium carbonate (6.45 g, 46.7 mmol) were combined with ethanol (50 mL). The mixture was refluxed for 3 hrs and filtered. The filtered solid was rinsed with ethanol (30 mL). The combined ethanol solution was evaporated to give a crude oily mixture which was purified by ISCO flash column chromatography (30% to 100% ethyl acetate in hexanes) to give N-(2-methylsulfanyl-pyrimidin-4-yl)-hydrazine as a white solid (2.8 g, 57.6% yield).

Источник