반응 #216657

반응 방정식

4-hydroxy-5-iodo-6-ethylpyrimidine

phosphorus oxychloride

phosphorus oxychloride

→

crystalline crude product

4-chloro-5-iodo-6-ethylpyrimidine

반응 조건

후처리

1. 1
   기타a slightly exothermic reaction
2. 2
   기타is kept constant at 60° C.
3. 3
   기타the reaction
4. 4
   workup.ADDITIONThe mixture is then poured onto ice-water
5. 5
   추출Extraction with ethyl acetate

실험 절차

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.

출처