반응 #1340246

ord-c60b2dbf423c48bab2f052f61203a80f

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 5 hours
  4. 4
    workup.WAITat 50° C. for 25 hours
  5. 5
    추출extracted with ethyl acetate
  6. 6
    추출The organic extract
  7. 7
    세척was washed with water
  8. 8
    건조dried over magnesium sulfate
  9. 9
    기타evaporated under reduced pressure
  10. 10
    기타The residue was triturated in diisopropyl ether

실험 절차

To a solution of 6-(3,4-dimethoxyphenyl)-3-methyl-2,4(1H,3H)-pyrimidinedione (3.0 g) in N,N-dimethylformamide (30 ml) was added sodium hydride (60% oil suspension, 0.50 g). The mixture was heated at 60° C. with stirring for 20 minutes and cooled to ambient temperature. To the mixture was added isopropyl bromide (15 ml) with stirring, which was continued at ambient temperature for 5 hours, and at 50° C. for 25 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 in diisopropyl ether to give 6-(3,4-dimethoxyphenyl)-2-isopropoxy-3-methyl-4(3H)-pyrimidinone (2.73 g).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04746664uspto-grants-1988_05