反応 #362874

ord-d212d5643d064c1aa8b036da5f204475

溶媒

反応条件

温度
70°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他is consumed
  2. 2
    温度The reaction is then cooled to room temperature
  3. 3
    洗浄washed 3 times with 10 ml saturated brine
  4. 4
    乾燥dried over MgSO4, and condensed in vacuo
  5. 5
    その他The crude product is purified by flash chromatography
  6. 6
    その他to afford 3

実験手順

A mixture of 2 (1 mmol), 3-aminoheptane (1.2 mmol), Pd2(DBA)3 (0.02 mol, 4 mol % Pd, 18 mg), BINP (0.04 mmol, 25 mg), NaOtBu (1.4 mmol, 134 mg), and toluene (0.11 M with 3-bromopyridine, 9 ml) is heated to 70° C. under nitrogen until 2 is consumed. The reaction is then cooled to room temperature, and taken up in 10 ml diethyl ether, washed 3 times with 10 ml saturated brine, dried over MgSO4, and condensed in vacuo . The crude product is purified by flash chromatography to afford 3.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06352990B1uspto-grants-2002_03