反応 #425376

ord-224e3bf9265a4f89af84305e57e62f38

反応条件

温度
110°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.ADDITIONwas added
  2. 2
    濃縮The reaction mixture was concentrated in half
  3. 3
    温度cooled to 0° C
  4. 4
    その他The precipitate that formed
  5. 5
    ろ過was collected by vacuum filtration
  6. 6
    洗浄The off-white solid was washed with hexanes

実験手順

The above compound, N-formyl-2-amino-3′,5-di-t-butyl biphenyl (6.5 g, 21 mmol) was dissolved into 50 mL of chlorobenzene to which 5 equivalents of di-t-butyl peroxide was added. The reaction mixture was heated to 110° C. for 72 hours. The reaction mixture was concentrated in half and cooled to 0° C. The precipitate that formed was collected by vacuum filtration. The off-white solid was washed with hexanes to give 2,9-di-tert-butylphenanthridinone as determined by GCMS and not purified any further.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08889864B2uspto-grants-2014_11