反応 #339928

ord-cd322c10f5204b44b3db05953f0862af

溶媒

反応条件

温度
100°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度to cool to room temperature
  2. 2
    濃縮concentrated
  3. 3
    その他purified directly by flash chromatography on silica gel (AcOEt/hexane: 10/90→430/70)

実験手順

To a solution of 221 (358 mg, 1.68 mmol) in dry toluene (7 mL) was added tributyl(vinyl)tin (514 μL, 1.76 mmol) followed by Pd(PPh3)4 (97 mg, 0.084 mmol) and the reaction mixture was heated at 100° C. for 16 h in a sealed tube. Then, the reaction mixture was allowed to cool to room temperature, concentrated, and purified directly by flash chromatography on silica gel (AcOEt/hexane: 10/90→430/70) to afford the title compound 222 (containing tributyltin chloride).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07868204B2uspto-grants-2011_01