反応 #450411

ord-d3424a71969041afa9fef9b76eb52ea9

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他a reaction scheme
  2. 2
    その他a compound that is useful as a precursor in the preparation of Group I compounds
  3. 3
    workup.STIRRINGThe reaction mixture is stirred overnight at room temperature
  4. 4
    その他acetone is removed under vacuum
  5. 5
    workup.DISSOLUTIONThe residue is dissolved in water (10 ml)

実験手順

FIG. 2A illustrates a reaction scheme for preparing 2-(4-aminophenoxy)-2-methyl propionic acid, a compound that is useful as a precursor in the preparation of Group I compounds. In accordance with the scheme of FIG. 2A, 8 grams (g) (0.2 mol) of pulverized sodium hydroxide is added to a suspension of 5.28 g (0.035 mol) of p-acetamidophenol in 23 ml (0.4 mol) of acetone. The reaction mixture is stirred at room temperature for 1/2 hour. Subsequently, 3.58 g (0.03 mol) of chloroform is added dropwise over the course of 30 minutes. The reaction mixture is stirred overnight at room temperature and acetone is removed under vacuum. The residue is dissolved in water (10 ml), followed by acidification with 37% hydrochloric acid (HCl) to produce a pale yellow precipitate of 2-(4-acetaminophenoxy)-2-methyl propionic acid (5 g, 60% yield), crystallized from methanol, mp 69°-71° C.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05872282uspto-grants-1999_02