반응 #708705

ord-1f2d2e446e7d4318b122ccaa86d0e802

반응 조건

온도
60°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도cooled to ambient temperature
  2. 2
    workup.STIRRINGwith stirring
  3. 3
    workup.WAITwhich was continued at ambient temperature for 3.5 hours
  4. 4
    추출extracted with ethyl acetate
  5. 5
    추출The organic extract
  6. 6
    세척was washed with water
  7. 7
    건조dried over magnesium sulfate
  8. 8
    기타evaporated under reduced pressure
  9. 9
    기타The residue was triturated with a mixture of ethyl acetate and diisopropyl ether
  10. 10
    기타the resulting precipitates
  11. 11
    여과were collected by filtration

실험 절차

To a solution of 6-(3,4-dimethoxyphenyl)-3-methyl-2,4(1H,3H)-pyrimidinedione (1.0 g) in N,N-dimethylformamide (10 ml) was added sodium hydride (60% in oil, 0.17 g). The mixture was heated at 60° C. with stirring for 20 minutes and cooled to ambient temperature. To the mixture was added ethyl iodide (5 ml) with stirring, which was continued at ambient temperature for 3.5 hours. To the reaction mixture was added water, and extracted with ethyl acetate. The organic extract was washed with water, dried over magnesium sulfate and evaporated under reduced pressure. The residue was triturated with a mixture of ethyl acetate and diisopropyl ether and the resulting precipitates were collected by filtration to give 6-(3,4-dimethoxyphenyl)-2-ethoxy-3-methyl-4(3H)-pyrimidinone (0.18 g) as by-product.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04824851uspto-grants-1989_04