반응 #1502148

ord-20b444c2fcf446a1b4276ef0e7e5ec57

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도Reflux
  2. 2
    온도cool
  3. 3
    workup.DISSOLUTIONDissolve the residue
  4. 4
    기타obtained
  5. 5
    기타after removal of solvent under reduced pressure
  6. 6
    workup.ADDITIONin a mixture of benzene (50 cc) and ether (50 cc)
  7. 7
    세척wash the solution in turn with sodium carbonate solution, 10% aqueous sulfuric acid and water
  8. 8
    기타Remove the solvent
  9. 9
    기타by evaporation under reduced pressure

실험 절차

Reflux a mixture of 2-cetylcyclopentane-1,3-dione (10.1 g), 6-m-methoxyphenylhex-1-en-3-one (6.0 g) and 0.02% methanolic potassium hydroxide solution (120 cc) for 26 hours and then cool. Dissolve the residue obtained after removal of solvent under reduced pressure in a mixture of benzene (50 cc) and ether (50 cc), and wash the solution in turn with sodium carbonate solution, 10% aqueous sulfuric acid and water. Remove the solvent by evaporation under reduced pressure to obtain as residue crude 2-cetyl-2-(6-m-methoxyphenyl-3-oxohexyl)-1,3-cyclopentanedione (11.4 g).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04002746uspto-grants-1977_01