反応 #1779

ord-319ce102069542b08b0f9d0be725ed30

溶媒

反応条件

温度
45°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度cooled to ambient temperature
  2. 2
    その他The solvent was removed under reduced pressure
  3. 3
    洗浄MeOH(NH3) and eluted with same
  4. 4
    その他The solvent was removed under reduced pressure

実験手順

To a stirred solution of methyl 4-(4-chromanoyloxy)-2-methoxybenzoate (260 mg, 0.82 mmol) in THF:H2O (4 mL:0.8 mL) was added LiOH.H2O (172 mg, 4.1 mmol). The reaction was heated to 45° C. over 12 h and then cooled to ambient temperature. The solvent was removed under reduced pressure. The crude solid was passed through a small plug of silca gel packed in 90:10 CH2Cl2 :MeOH(NH3) and eluted with same. The solvent was removed under reduced pressure to afford 4-(4-chromanoyloxy)-2-methoxybenzoic acid as a foam.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05726172uspto-grants-1998_03