Reaktion #1172829

Reaktionsgleichung

4,6-di-fluoro-2-methylthiopyrimidine

hydrazine monohydrate

→

title compound

Ausbeute 94.7%

4-Fluoro-2-methylthio-6-hydrazinopyrimidine

Ausbeute 94.7%

Lösungsmittel

ethanol

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigethe temperature below 0° C.
2. 2
   Sonstigeto react for an additional 30 min
3. 3
   Sonstigethe volatiles were then removed by evaporation under reduced pressure
4. 4
   workup.ADDITIONThe residue was diluted with ethyl acetate
5. 5
   Extraktionthe resulting solution extracted with water
6. 6
   Trocknendried over magnesium sulfate
7. 7
   Einengenconcentrated under reduced pressure

Vorschrift

A solution of 15.8 g (0.097 mol) of 4,6-di-fluoro-2-methylthiopyrimidine in 50 ml of ethanol was added slowly with stirring to a solution of 11.6 ml (12.0 g, 0.214 mol) of hydrazine monohydrate in 100 ml of ethanol, keeping the temperature below 0° C. by external cooling. The mixture was allowed to react for an additional 30 min and the volatiles were then removed by evaporation under reduced pressure. The residue was diluted with ethyl acetate and the resulting solution extracted with water, dried over magnesium sulfate, and concentrated under reduced pressure to obtain 16.0 g of the title compound as a white powder melting at 153° C.-154° C.

Quelle