反応 #1253969

ord-c0acf37e673345a29bf4550df46cc2ac

試薬

なし

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他the reaction for one hour
  2. 2
    洗浄washed with water (3×), aqueous saturated NaHCO3 (2×) and brine
  3. 3
    乾燥dried over MgSO4
  4. 4
    濃縮concentrated
  5. 5
    その他The product was purified by silica gel column chromatography
  6. 6
    その他recrystallized from methanol
  7. 7
    その他to give yellow needles

実験手順

To a cold (0° C.) suspension of 1-methylnaphthalene (5 g) in HNO3 was added H2SO4 (5 mL) dropwise. After stirring the reaction for one hour, the solution was diluted with ethyl acetate and washed with water (3×), aqueous saturated NaHCO3 (2×) and brine, dried over MgSO4, and concentrated. The product was purified by silica gel column chromatography using ethyl acetate:hexane (5:95) and recrystallized from methanol to give yellow needles.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06613942B1uspto-grants-2003_09