反応 #310545

反応方程式

4-hydroxy-6-methyl-2-trichloromethylpyrimidine

triethylamine

ethyl chloroformate

→

4-Ethoxycarbonyloxy-6-Methyl-2-Trichloromethylpyrimidine

収率 67.0%

溶媒

ether

反応条件

後処理

1. 1
   温度The reaction mixture was refluxed for 2 hours
2. 2
   ろ過filtered
3. 3
   その他rotary evaporated under aspiration
4. 4
   その他to give a dark oil
5. 5
   その他This was triturated with petroleum ether
6. 6
   その他the solution decanted from tars
7. 7
   workup.DISTILLATIONthe product distilled
8. 8
   その他to give 2.7 g (67% yield; bp0.5 mm 125° C.)

実験手順

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.

出典