反応 #325662

ord-65cdf4843e424619bae027e2bf1b6106

溶媒

反応条件

温度
120°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他was degassed with nitrogen
  2. 2
    温度The next day, the reaction mixture was cooled to RT
  3. 3
    ろ過filtered
  4. 4
    濃縮concentrated in vacuo
  5. 5
    洗浄The crude was eluted on a silica gel column with 15% to 22% EtOAc/hexanes gradient system
  6. 6
    その他to yield a yellow-brown oil

実験手順

A mix of 1-(tert-butyl)-2-bromo-4-nitrobenzene (3.652 g), TEA (5.92 ml), 3-buten-1-ol (5.48 ml), Pd(OAc)2 (32 mg), Pd(PPh3)4 (327 mg) and toluene (40 ml) was degassed with nitrogen and heated in a sealed vessel for 16 h at 120° C. The next day, the reaction mixture was cooled to RT, filtered, and concentrated in vacuo. The crude was eluted on a silica gel column with 15% to 22% EtOAc/hexanes gradient system to yield a yellow-brown oil.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08642624B2uspto-grants-2014_02