반응 #648621

ord-ad9fdb94f25a41c49ada9fd2b5315077

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The reaction mixture was heated
  2. 2
    온도under reflux for 4 h
  3. 3
    농축It was concentrated
  4. 4
    기타the crude product was purified firstly by flash chromatography on silica gel (mobile phase: cyclohexane/ethyl acetate gradient)

실험 절차

17 mg (271 μmol) of copper powder were added to a solution of 2.66 g (5.43 mmol) of the compound from Example 97A in 10 ml of pyridine and 2 ml of ethanol. The reaction mixture was heated under reflux for 4 h. It was concentrated, and the crude product was purified firstly by flash chromatography on silica gel (mobile phase: cyclohexane/ethyl acetate gradient) and then by preparative HPLC (mobile phase: acetonitrile/water gradient). 1.73 g (74% of theory) of the title compound were obtained.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08063234B2uspto-grants-2011_11