反応 #2179583

ord-18c6ca74cde142128b7c2aebd19ed90d

試薬

なし

反応条件

温度
85°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度to cool to RT
  2. 2
    濃縮concentrated
  3. 3
    workup.ADDITIONThe residue was diluted in H2O
  4. 4
    抽出extracted with DCM
  5. 5
    洗浄The organic phase was washed with H2O
  6. 6
    乾燥dried (Na2SO4)
  7. 7
    ろ過filtered
  8. 8
    濃縮concentrated

実験手順

A mixture of homovanillic acid (5 g, 27.4 mmol) and H2SO4 (96%, 1.46 mL, 27.4 mmol) in EtOH (100 mL) was stirred for 1 h at 85° C., allowed to cool to RT and concentrated. The residue was diluted in H2O and extracted with DCM. The organic phase was washed with H2O, dried (Na2SO4), filtered and concentrated to afford 5.8 g of the title compounds as a yellow oil. LC-MS: m/z 211.2 [M+H]+.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08440693B2uspto-grants-2013_05