반응 #310545

반응 방정식

4-hydroxy-6-methyl-2-trichloromethylpyrimidine

triethylamine

ethyl chloroformate

→

4-Ethoxycarbonyloxy-6-Methyl-2-Trichloromethylpyrimidine

수율 67.0%

용매

ether

반응 조건

후처리

1. 1
   온도The reaction mixture was refluxed for 2 hours
2. 2
   여과filtered
3. 3
   기타rotary evaporated under aspiration
4. 4
   기타to give a dark oil
5. 5
   기타This was triturated with petroleum ether
6. 6
   기타the solution decanted from tars
7. 7
   workup.DISTILLATIONthe product distilled
8. 8
   기타to give 2.7 g (67% yield; bp0.5 mm 125° C.)

실험 절차

To a solution of 3.0 g (0.013 mole) 4-hydroxy-6-methyl-2-trichloromethylpyrimidine, 1.4 g (0.013 mole) triethylamine, and 75 ml ether was added 1.4 g (0.013 mole) ethyl chloroformate. The reaction mixture was refluxed for 2 hours, filtered, and rotary evaporated under aspiration to give a dark oil. This was triturated with petroleum ether and the solution decanted from tars. The solvent was stripped in vacuo and the product distilled to give 2.7 g (67% yield; bp0.5 mm 125° C.). The structure was confirmed via infrared and elemental analysis.

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