반응 #310546

ord-202ff74c73484d83a6760d7d4ea508eb

반응 방정식

Cc1cc(O)nc(C(Cl)(Cl)Cl)n1
4-hydroxy-6-methyl-2-trichloromethylpyrimidine
CCN(CC)CC
triethylamine
CCOCC
ether
CC(C)OC(=O)Cl
isopropyl chloroformate
Cc1cc(OC(=O)OC(C)C)nc(C(Cl)(Cl)Cl)n1
product
수율 58.9%
Cc1cc(OC(=O)OC(C)C)nc(C(Cl)(Cl)Cl)n1
4-Isopropoxycarbonyloxy-6-Methyl-2-Trichloromethylpyrimidine
수율 58.9%

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The reaction mixture was refluxed one hour
  2. 2
    여과filtered
  3. 3
    기타rotary evaporated
  4. 4
    기타to give a yellow oil
  5. 5
    workup.DISTILLATIONThe oil was distilled (bp1.2 mm 120° C.)
  6. 6
    기타to give a cloudy yellow oil
  7. 7
    여과filtered
  8. 8
    기타the solvent removed

실험 절차

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 1.6 g (0.013 mole) isopropyl chloroformate. The reaction mixture was refluxed one hour, filtered, and rotary evaporated to give a yellow oil. The oil was distilled (bp1.2 mm 120° C.) to give a cloudy yellow oil. This was taken up in benzene, filtered, and the solvent removed leaving 2.4 g (57% yield) of product. The structure was confirmed via infrared and elemental analysis.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04353908uspto-grants-1982_10