Reaktion #70245

Reaktionsgleichung

4-chloro-2-methylsulfanyl-pyrimidine

hydrazine

potassium carbonate

→

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

Ausbeute 57.6%

Lösungsmittel

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe mixture was refluxed for 3 hrs
2. 2
   Filtrationfiltered
3. 3
   WaschenThe filtered solid was rinsed with ethanol (30 mL)
4. 4
   SonstigeThe combined ethanol solution was evaporated
5. 5
   Sonstigeto give a crude oily mixture which
6. 6
   Sonstigewas purified by ISCO flash column chromatography (30% to 100% ethyl acetate in hexanes)

Vorschrift

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).

Quelle