反応 #310320

反応方程式

4-hydroxy-6-methyl-2-trichloromethylpyrimidine

triethylamine

crotonyl chloride

→

pure product

収率 45.0%

4-Crotonoxy-6-Methyl-2-Trichloromethylpyrimidine

収率 45.0%

溶媒

diethyl ether

—

petroleum ether

反応条件

後処理

1. 1
   温度The reaction mixture was refluxed for 15 hours
2. 2
   ろ過filtered
3. 3
   濃縮the filtrate was concentrated in-vacuo
4. 4
   その他to give a viscous oil as residue
5. 5
   その他Recrystallization from isopropyl alcohol

実験手順

To a solution of 3.0 g (0.02 mole) 4-hydroxy-6-methyl-2-trichloromethylpyrimidine and 1.3 g (0.02 mole) triethylamine in 75 ml diethyl ether was added 1.4 g (0.02 mole) crotonyl chloride. The reaction mixture was refluxed for 15 hours and filtered, and the filtrate was concentrated in-vacuo to give a viscous oil as residue. Trituration with petroleum ether caused the oil to solidify. Recrystallization from isopropyl alcohol gave 1.8 g (45% yield) of pure product; m.p. 55° C.

出典