反応 #84543

ord-74a1e08e410b41e390b42a7a8940f57f

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    抽出extracted with DCM (20 mL×2)
  2. 2
    洗浄The combined organic layers were washed with brine (40 mL×2)
  3. 3
    乾燥dried over anhydrous Na2SO4
  4. 4
    濃縮concentrated in vacuo
  5. 5
    その他The residue was purified by a silica gel column chromatography (EtOAc)

実験手順

To a solution of NaOH (4.89 g, 122 mmol) in a mixture of water (20 mL) and MeOH (20 mL) in an ice bath was added a solution of ethyl 2-(cyclohexyloxy)acetate (3.8 g, 20.4 mmol) in MeOH (10 mL) slowly and the mixture was stirred at rt for 2 h. It was then acidified to pH 4 with concentrated hydrochloric acid and extracted with DCM (20 mL×2). The combined organic layers were washed with brine (40 mL×2), dried over anhydrous Na2SO4 and concentrated in vacuo. The residue was purified by a silica gel column chromatography (EtOAc) to give the title compound as pale yellow oil (2.7 g, 84%).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US09434695B2uspto-grants-2016_09