반응 #1340241

ord-b5bff3d9b96c4359a14d4905ecc492f6

반응 조건

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

후처리

  1. 1
    온도cooled to 0° C
  2. 2
    workup.STIRRINGwith stirring
  3. 3
    workup.WAITwhich was continued at 0° C. for 2 hours and at ambient temperature for 3 hours
  4. 4
    추출the reaction mixture was extracted 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 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 (3.0 g) in N,N-dimethylformamide (30 ml) was added sodium hydride (60% in oil, 0.5 g). The mixture was heated at 60° C. with stirring for 20 minutes and cooled to 0° C. To the mixture was added n-propyl iodide (15 ml) with stirring, which was continued at 0° C. for 2 hours and at ambient temperature for 3 hours. After addition of water, the reaction mixture was 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 diisopropyl ether and the resulting precipitates were collected by filtration to give 6-(3,4-dimethoxyphenyl)-3-methyl-2-propoxy-4(3H)-pyrimidinone (1.15 g) as byproduct.

출처

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