Phosphorus oxychloride → 105950-89-8

Participants

Reaction Conditions

Reaction Steps

47 g (335.7 mmol) of 4-hydroxy-2-methoxymethylpyrimidine (from stage a) are mixed with 210 ml of phosphorus oxychloride and stirred at 70° C. for 2 h and subsequently heated to boiling for 2.5 h. The excess phosphorus oxychloride is removed by distillation in vacuo, the residue is hydrolyzed with ice, and solid potassium bicarbonate is added to eliminate excess acid. Several extractions with methylene chloride are carried out, and the organic phase is evaporated in vacuo. The black residue is filtered through silica gel (n-heptane/ethyl acetate 1:1). 15.7 g of oil are obtained.

Provenance & Evidence