反応 #997335

ord-3cc29f8d70a3412da177b0704bc0ea63

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度the mixture heated for 2 hours
  2. 2
    濃縮After concentration in vacuo the residue
  3. 3
    その他was purified by flash chromatography

実験手順

Methyl 8-chloro-6-oxo-2,3,4,6-tetrahydro-1H-quinolizine-9-carboxylate (7b, 1.23 g, 5.1 mmol, 1 eq) was dissolved in DMF (10 ml) at 88° C. Selectfluor (3.61 g, 10.2 mmol, 2 eq) in DMF (10 ml) was added drop wise and the mixture heated for 2 hours. After concentration in vacuo the residue was purified by flash chromatography using 20-70% EtOAc/Hexane as eluent to give the title compound as an off-white solid (600 mg, 45%). [M+H] calc'd for C11H11ClFNO3, 260. found, 260

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08022057B2uspto-grants-2011_09