Phosphorus oxychloride → 4-Chloro-6-ethyl-5-iodopyrimidine

関与物質

反応条件

反応手順

21.7 g (0.087 mol) of 4-hydroxy-5-iodo-6-ethylpyrimidine are stirred into 50 ml of phosphorus oxychloride which has been heated to 60° C., a slightly exothermic reaction taking place. The temperature is kept constant at 60° C. and the mixture is left for one hour to complete the reaction. The mixture is then poured onto ice-water and stirred for 30 minutes in order to hydrolyse completely the excess phosphorus oxychloride. Extraction with ethyl acetate yields 23.5 g of crystalline crude product. Recrystallisation from a mixture of 1 part ethyl acetate and 10 parts hexane yields 18.8 g (80.7% of the theoretical yield) of pure substance; m.p. 56°-57° C.

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