반응 #168587

ord-a010378496ce4d479c7bed4cc77af8c5

용매

반응 조건

온도
50°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도the reaction mixture heated at 50° C. for 24 hours
  2. 2
    여과After hot filtration
  3. 3
    기타the filtrate is evaporated to dryness under reduced pressure
  4. 4
    기타The obtained oil is further purified by silica-gel flash chromatography

실험 절차

A mixture of 6-chloro-3-methylpyrimidine-2,4(1H,3H)-dione (3 g, 18.8 mmol), isobutyl iodide (5 mL, 43.5 mmol) and potassium carbonate (5.3 g, 38.4 mmol) in anhydrous DMF (200 mL) is heated at 50° C. for 8 hours. Additional isobutyl iodide (4.3 mL, 37.5 mmol) is added, and the reaction mixture heated at 50° C. for 24 hours. After hot filtration, the filtrate is evaporated to dryness under reduced pressure. The obtained oil is further purified by silica-gel flash chromatography to give 2.1 g of pure product (Yield: 52%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08846693B2uspto-grants-2014_09