反応 #73064

ord-d0e8a8134ece44b5b765280cd6098265

反応条件

温度
90°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度was heated
  2. 2
    温度The reaction mixture was cooled to 50° C.
  3. 3
    ろ過The resulting precipitate was filtered
  4. 4
    洗浄washed with water
  5. 5
    その他dried over vacuum for 3 days

実験手順

A mixture of 7-bromo[1,5]naphthyridin-4-ol (33 g, 0.147 mol) and fuming nitric acid (350 mL) was heated at reflux (90° C. internal reaction vessel temperature) for 3 hours. The reaction mixture was cooled to 50° C., poured over 1 L of ice and neutralized to pH 2-3 with a solution of 50% aqueous NaOH. The resulting precipitate was filtered, washed with water, and dried over vacuum for 3 days to yield 25.1 g of 7-bromo-3-nitro[1,5]naphthyridin-4-ol as a yellow crystalline solid.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08541438B2uspto-grants-2013_09