반응 #310320

ord-862eea4fe61a46a7a4bd37ce9962335e

반응 방정식

Cc1cc(O)nc(C(Cl)(Cl)Cl)n1
4-hydroxy-6-methyl-2-trichloromethylpyrimidine
CCN(CC)CC
triethylamine
C/C=C/C(=O)Cl
crotonyl chloride
C/C=C/C(=O)Oc1cc(C)nc(C(Cl)(Cl)Cl)n1
pure product
수율 45.0%
C/C=C/C(=O)Oc1cc(C)nc(C(Cl)(Cl)Cl)n1
4-Crotonoxy-6-Methyl-2-Trichloromethylpyrimidine
수율 45.0%

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The reaction mixture was refluxed for 15 hours
  2. 2
    여과filtered
  3. 3
    농축the filtrate was concentrated in-vacuo
  4. 4
    기타to give a viscous oil as residue
  5. 5
    기타Recrystallization 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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04352806uspto-grants-1982_10