반응 #95002
ord-e649a692c4fb41879d7c7deb50b8f5d0
반응 방정식
4-hydroxy-6-methyl-2-trichloromethylpyrimidine
potassium carbonate
dimethylcarbamoyl chloride
acetone
→
residue
6-Methyl-2-Trichloromethyl-4-Pyrimidinyl Diethylcarbamate
반응물
시약
없음
반응 조건
상세 조건
See reaction.notes.procedure_details.
후처리
- 1온도was refluxed 5 hours
- 2여과A precipitate was filtered out
- 3기타the filtrate rotary evaporated
실험 절차
A mixture of 5.8 g (0.027 mole) 4-hydroxy-6-methyl-2-trichloromethylpyrimidine, 3.3 g (0.024 mole) potassium carbonate, 3.3 g (0.024 mole) dimethylcarbamoyl chloride, and 100 ml acetone was refluxed 5 hours. A precipitate was filtered out and the filtrate rotary evaporated to give 10.2 g residue. This was taken up in chloroform, the solution washed with 1% sodium hydroxide, water, and dried over anhydrous magnesium sulfate. Rotary evaporation yielded 5.2 g residue which was recrystallized from petroleum ether to give 2.1 g (24% yield) of product. An analytical sample recrystallized a second time from petroleum ether had mp 77°-77.5° C. The structure was confirmed via infrared and elemental analysis.