反応 #47807

ord-eb586fb93bd04fb89fa2dcf248ee2585

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    洗浄The resulting mixture washed with saturated ammonium chloride
  2. 2
    抽出extracted with ethyl acetate
  3. 3
    その他The organic layer was separated
  4. 4
    乾燥dried over anhydrous MgSO4
  5. 5
    濃縮concentrated under a reduced pressure
  6. 6
    その他Then, the resulting residue was purified by flash chromatography

実験手順

6-Hydroxy-1-oxo-3-phenyl-1H-indene-2-carboxylic acid ethyl ester (2 g, 6.79 mmol) prepared in Preparation Example 2, potassium carbonate (1.40 g, 10.19 mmol) and sodium iodide (0.2 g, 1.39 mmol) were dissolved in N,N-dimethyl formamide, and 1-bromo-3-phenyl propane (2.066 ml, 13.592 mmol) was added thereto, followed by stirring for 8 hrs at room temperature. The resulting mixture washed with saturated ammonium chloride and extracted with ethyl acetate. The organic layer was separated, dried over anhydrous MgSO4, and concentrated under a reduced pressure. Then, the resulting residue was purified by flash chromatography to obtain 2.37 g of the titled compound (yield: 85%) as a dark red solid.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07745439B2uspto-grants-2010_06