反応 #61659

ord-77418d8c43974fee8734f31649c38fcb

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度The mixture is refluxed for 30 minutes
  2. 2
    ろ過The solid is filtered off
  3. 3
    洗浄washed with dioxane
  4. 4
    workup.DISSOLUTIONdissolved in 600 mL dichloromethane/methanol (9:1)
  5. 5
    洗浄The solution is washed with sodium hydrogen carbonate solution
  6. 6
    乾燥dried with sodium sulphate
  7. 7
    その他evaporated down
  8. 8
    ろ過filtered
  9. 9
    その他dried

実験手順

13.0 g (44 mmol) 5-acetyl-7-benzyloxy-3,4-dihydro-1H-quinolin-2-one are suspended in 130 mL dioxane and combined with 15.0 g (66 mmol) of 2,3-dichloro-5,6-dicyanobenzoquinone. The mixture is refluxed for 30 minutes, cooled to ambient temperature and stirred for a further 2 hours. The solid is filtered off, washed with dioxane and dissolved in 600 mL dichloromethane/methanol (9:1). The solution is washed with sodium hydrogen carbonate solution, dried with sodium sulphate and evaporated down. Then the residue is suspended in methanol, filtered and dried.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07429583B2uspto-grants-2008_09