Reaktion #1438792

Reaktionsgleichung

4-hydroxy-2-(methylthio)pyrimidine-5-carbonitrile

POCl3

→

title compound

4-chloro-2-(methylthio)pyrimidine-5-carbonitrile

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturto reflux for 2 h
2. 2
   EinengenThe reaction mixture was concentrated in vacuo
3. 3
   Sonstigethe residue quenched with ice (100 g)
4. 4
   Extraktionextracted with ethyl acetate (3×50 mL)
5. 5
   WaschenThe combined ethyl acetate layers were washed with water (20 mL), brine (10 mL)
6. 6
   Trocknendried over Na2SO4
7. 7
   Filtrationfiltered
8. 8
   Einengenconcentrated

Vorschrift

A stirred solution of 4-hydroxy-2-(methylthio)pyrimidine-5-carbonitrile (British patent GB901749) (1.00 g, 5.98 mmol) in POCl3 (5 mL) was heated to reflux for 2 h. The reaction mixture was concentrated in vacuo and the residue quenched with ice (100 g). The solution was then basified to pH 8 with sat. aq NaHCO3 and extracted with ethyl acetate (3×50 mL). The combined ethyl acetate layers were washed with water (20 mL), brine (10 mL), dried over Na2SO4, filtered and concentrated to give the title compound.

Quelle