반응 #95002

ord-e649a692c4fb41879d7c7deb50b8f5d0

반응 방정식

Cc1cc(O)nc(C(Cl)(Cl)Cl)n1
4-hydroxy-6-methyl-2-trichloromethylpyrimidine
O=C([O-])[O-].[K+].[K+]
potassium carbonate
CN(C)C(=O)Cl
dimethylcarbamoyl chloride
CC(C)=O
acetone
CCN(CC)C(=O)Oc1cc(C)nc(C(Cl)(Cl)Cl)n1
residue
CCN(CC)C(=O)Oc1cc(C)nc(C(Cl)(Cl)Cl)n1
6-Methyl-2-Trichloromethyl-4-Pyrimidinyl Diethylcarbamate

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도was refluxed 5 hours
  2. 2
    여과A precipitate was filtered out
  3. 3
    기타the filtrate rotary evaporated

실험 절차

A mixture of 5.8 g (0.027 mole) 4-hydroxy-6-methyl-2-trichloromethylpyrimidine, 3.3 g (0.024 mole) potassium carbonate, 3.3 g (0.024 mole) dimethylcarbamoyl chloride, and 100 ml acetone was refluxed 5 hours. A precipitate was filtered out and the filtrate rotary evaporated to give 10.2 g residue. This was taken up in chloroform, the solution washed with 1% sodium hydroxide, water, and dried over anhydrous magnesium sulfate. Rotary evaporation yielded 5.2 g residue which was recrystallized from petroleum ether to give 2.1 g (24% yield) of product. An analytical sample recrystallized a second time from petroleum ether had mp 77°-77.5° C. The structure was confirmed via infrared and elemental analysis.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04343803uspto-grants-1982_08