反応 #2185247

ord-db6aabb438794ed584b303e69c409ae4

溶媒

反応条件

温度
150°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    濃縮was concentrated under reduced pressure
  2. 2
    その他the residue purified by flash chromatography

実験手順

9-Bromothieno[3,2-e][1,2,4]triazolo[1,5-c]pyrimidine (1.16 g, 4.55 mmol) was dissolved in DMF (23 mL), and copper(I) cyanide (817 mg, 9.1 mmol) was added. This mixture was heated to 150° C. for 23 h, whereupon the reaction mixture was concentrated under reduced pressure, and the residue purified by flash chromatography. LCMS method [4], retention time=0.890 min; MS (ESI) 202.0 (MH+); 1H NMR (300 MHz, CDCl3) δ 9.36 (s, 1H), 8.57 (s, 1H), 8.32 (s, 1H).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08450363B2uspto-grants-2013_05