반응 #94995

ord-edb09a750cee4f589a429a93eeee7555

반응 방정식

Cc1cc(O)nc(C(Cl)(Cl)Cl)n1
4-hydroxy-6-methyl-2-trichloromethylpyrimidine
CCN(CC)CC
triethylamine
CN(C)C(=O)Cl
dimethylcarbamoyl chloride
Cc1cc(OC(=O)N(C)C)nc(C(Cl)(Cl)Cl)n1
6-Methyl-2-Trichloromethyl-4-Pyrimidinyl Dimethylcarbamate
수율 48.0%

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.STIRRINGThe reaction mixture was stirred 2 hours
  2. 2
    온도under reflux
  3. 3
    온도to cool
  4. 4
    여과A solid was filtered out
  5. 5
    온도after cooling
  6. 6
    세척washed with water
  7. 7
    기타to give 3.6 g (48% yield; mp 83.5°-84.5° C.)

실험 절차

A mixture of 5.7 g (0.025 mole) 4-hydroxy-6-methyl-2-trichloromethylpyrimidine, 5.1 g (0.05 mole) triethylamine, and 100 ml acetonitrile was stirred and 5.4 g (0.05 mole) dimethylcarbamoyl chloride was added to the mixture. The reaction mixture was stirred 2 hours under reflux, and allowed to cool. A solid was filtered out after cooling and washed with water to give 3.6 g (48% yield; mp 83.5°-84.5° C.). The structure was confirmed via infrared and elemental analysis.

출처

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