반응 #310542

ord-a816d89191784e31b884dd383ca127b3

반응 방정식

Cc1cc(O)nc(C(Cl)(Cl)Cl)n1
4-hydroxy-6-methyl-2-trichloromethylpyrimidine
CCN(CC)CC
triethylamine
O=C(Cl)Oc1ccccc1
phenyl chloroformate
Cc1cc(OC(=O)Oc2ccccc2)nc(C(Cl)(Cl)Cl)n1
thick oily residue
수율 94.9%
Cc1cc(OC(=O)Oc2ccccc2)nc(C(Cl)(Cl)Cl)n1
6-Methyl-4-Phenoxycarbonyloxy-2-Trichloromethylpyrimidine
수율 94.9%

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The solution refluxed on addition
  2. 2
    기타a precipitate formed
  3. 3
    여과filtered
  4. 4
    기타the filtrate rotary evaporated

실험 절차

To 5.6 g (0.02 mole) 4-hydroxy-6-methyl-2-trichloromethylpyrimidine, 2.0 g (0.02 moles) triethylamine, and 100 ml ether was added 3.2 g (0.07 mole) phenyl chloroformate. The solution refluxed on addition and a precipitate formed. This was stirred 0.5 hour, filtered, and the filtrate rotary evaporated to give 6.6 g (76% yield) thick oily residue. Extraction with ligroin gave, on cooling of the extract, 3.7 g pure product as a viscous oil. The structure was confirmed via infrared and elemental analysis.

출처

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