반응 #310320
ord-862eea4fe61a46a7a4bd37ce9962335e
반응 방정식
4-hydroxy-6-methyl-2-trichloromethylpyrimidine
triethylamine
crotonyl chloride
→
pure product
수율 45.0%
4-Crotonoxy-6-Methyl-2-Trichloromethylpyrimidine
수율 45.0%
반응 조건
상세 조건
See reaction.notes.procedure_details.
후처리
- 1온도The reaction mixture was refluxed for 15 hours
- 2여과filtered
- 3농축the filtrate was concentrated in-vacuo
- 4기타to give a viscous oil as residue
- 5기타Recrystallization from isopropyl alcohol
실험 절차
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.