反応 #6908

ord-d57d16896f9f4187ad5a58a2a543f654

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    ろ過the reaction was filtered through CELITE diatomaceous earth
  2. 2
    洗浄washed copiously with methanol
  3. 3
    その他The volatiles were removed under vacuum
  4. 4
    その他the crude residue was triturated with ether
  5. 5
    その他The solids were collected on a fritted funnel
  6. 6
    その他dried under vacuum

実験手順

3,4-Dihydroquinolin-2(1H)-one (7.5 g; 51 mmol) and silver (I) sulfate (17.5 g; 56.1 mmol) were suspended in ethanol (250 mL). A solution of iodine in ethanol (250 mL) was added slowly to the reaction over 1 hour. After 6 hours, the reaction was filtered through CELITE diatomaceous earth and washed copiously with methanol. The volatiles were removed under vacuum and the crude residue was triturated with ether. The solids were collected on a fritted funnel and dried under vacuum. This provided the title compound.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07084156B2uspto-grants-2006_08