반응 #94996

반응 방정식

4-hydroxy-6-methyl-2-trichloromethylpyrimidine

triethylamine

diphenylcarbamoyl chloride

→

residue

수율 88.0%

6-Methyl-2-Trichloromethyl-4-Pyrimidinyl Diphenylcarbamate

수율 88.0%

용매

acetonitrile

반응 조건

후처리

1. 1
   온도The reaction mixture was refluxed 4 hours
2. 2
   여과A precipitate was filtered out and ether
3. 3
   workup.ADDITIONwas added to the filtrate
4. 4
   기타yielding more precipitate
5. 5
   기타Rotary evaporation

실험 절차

To a mixture of 5.7 g (0.025 mole) 4-hydroxy-6-methyl-2-trichloromethylpyrimidine, 2.6 g (0.025 mole) triethylamine, and 100 ml acetonitrile was added 5.8 g (0.025 mole) diphenylcarbamoyl chloride. The reaction mixture was refluxed 4 hours. A precipitate was filtered out and ether was added to the filtrate yielding more precipitate. Rotary evaporation gave 9.3 g residue which was recrystallized from ligroin to give 6.15 g (58% yield) of product. An analytical sample was recrystallized a second time from ligroin and had mp 132°-134° C. The structure was confirmed via infrared and elemental analysis.

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