Yield:3740-82-7 70%

Reaction Conditions:

with trichlorophosphate at 100; for 48 h;Green chemistry;

Steps:

General Scale Up Procedure for the 2-Substituted 4,6-Dichloropyrimidines 5

General procedure: To 40 g of the 2-substituted 6-hydroxy-[3H]-pyrimidin-4-one 4, 300 mL of phosphoryl chloride was added. The mixture was heated for 48 h at 100°C. The excess of phosphoryl chloride was removed by distillation under reduced pressure (20 mbar). Chloroform (200 mL) and ice water (100 mL) were added and the mixture was well stirred for 30 min. The solution was adjusted to pH 5-6 with aqueous sodium carbonate solution. The organic layer was separated and the water phase was extracted three times with 200 mL of chloroform. The combined chloroform phases were dried with magnesium sulfate, filtered, and finally the chloroform was removed under reduced pressure. The obtained crude material was distilled under reduced pressure or purified by column chromatography using silica gel, mesh 60, and chloroform.

References:

Opitz, Andreas;Sulger, Werner;Daltrozzo, Ewald;Koch, Rainer [Australian Journal of Chemistry,2015,vol. 68,# 5,p. 814 - 824]