反応 #94996

反応方程式

4-hydroxy-6-methyl-2-trichloromethylpyrimidine

triethylamine

diphenylcarbamoyl chloride

→

residue

収率 88.0%

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

収率 88.0%

溶媒

acetonitrile

反応条件

後処理

1. 1
   温度The reaction mixture was refluxed 4 hours
2. 2
   ろ過A precipitate was filtered out and ether
3. 3
   workup.ADDITIONwas added to the filtrate
4. 4
   その他yielding more precipitate
5. 5
   その他Rotary evaporation

実験手順

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.

出典