反応 #47804

ord-2d115b5c4e044e0196e1005cb6e5473b

溶媒

反応条件

温度
0°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    洗浄The resulting mixture washed with saturated saline
  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The resulting residue was purified by flash chromatography

実験手順

6-Methoxy-1-oxo-3-phenyl-1H-indene-2-carboxylic acid ethyl ester (300 mg, 0.974 mmol) obtained in Example 1 was dissolved in THF and 1.2 equivalents of methylmagnesium chloride were added thereto, followed by stirring for 3 hrs at 0° C. The resulting mixture washed with saturated saline and extracted with ethyl acetate. The organic layer was separated, dried over anhydrous MgSO4, and concentrated under a reduced pressure. The resulting residue was purified by flash chromatography to obtain 126 mg of the titled compound (yield: 38%).

出典

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