反応 #77737

ord-e2da5b6fc92c4373bfb43f28abe30963

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    ろ過The reaction mixture is filtered
  2. 2
    濃縮the filtrate is concentrated in vacuo
  3. 3
    workup.DISSOLUTIONThe resultant residue is dissolved in ethyl acetate
  4. 4
    洗浄washed with saturated aqueous NaHCO3
  5. 5
    乾燥The organic phase is dried over MgSO4
  6. 6
    濃縮concentrated in vacuo

実験手順

A solution of ethyl 7-amino-4-oxo-4H-chromene-2-carboxylate (1.00 g, 4.3 mmol) in ethanol and concentrated HCl (5 mL) is hydrogenated over 10% Pd/C (0.5 g) at 50 psi for 72 h at ambient temperature. The reaction mixture is filtered and the filtrate is concentrated in vacuo. The resultant residue is dissolved in ethyl acetate and washed with saturated aqueous NaHCO3. The organic phase is dried over MgSO4, and concentrated in vacuo to afford the title compound as an amber oil, 0.85 g (89% yield), identified by NMR and mass spectral analyses.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06706757B2uspto-grants-2004_03