反応 #69601

ord-fb7dc96696914466a7ba71ba17802332

反応条件

温度
120°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.STIRRINGThe resulting mixture was stirred for additional 2 hr at 120° C
  2. 2
    workup.STIRRINGthe reaction mixture was stirred for 2 hr at 120° C
  3. 3
    その他Finally, the product was isolated

実験手順

A mixture of 4.75 g (33 mmol) of 8-aminoquinoline, 3.03 g (30 mmol) of triethylamine and 7.85 g (30 mmol) of 6 was stirred for 2 hr at 120° C. One more portion of 3.03 g of triethylamine as well as 7.85 g of 6 was added. The resulting mixture was stirred for additional 2 hr at 120° C. Next, one more portion of triethylamine and 6 were added, and the reaction mixture was stirred for 2 hr at 120° C. Finally, the product was isolated using flash chromatography on silica gel 60 (40-63 um, eluent: hexanes-ethyl acetate=20:1, vol.). Yield 2.78 g (26%).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08530593B2uspto-grants-2013_09