反応 #90092

ord-f865c7d0fe7f44da81d69c156db8f76c

溶媒

反応条件

温度
80°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    抽出extracted with ethyl acetate
  2. 2
    抽出extracted with ethyl acetate
  3. 3
    洗浄washed with saturated brine
  4. 4
    乾燥dried over sodium sulfate
  5. 5
    その他The drying agent was removed by filtration
  6. 6
    その他the residues obtained
  7. 7
    濃縮after concentration under reduced pressure
  8. 8
    その他were purified by silica gel column chromatography (ethyl acetate/hexane)
  9. 9
    その他to obtain the target compound (white solid, 1.10 g, 84%)

実験手順

2-(4-Isopropoxy-3-methoxy-phenyl)-2-methyl-propionic acid ethyl ester (Compound L3-1, 1.45 g, 5.17 mmol) was dissolved in THF (13 mL) and EtOH (13 mL), added with 1 N aqueous solution of sodium hydroxide (10.3 mL, 2.0 eq.), and stirred at 80° C. overnight. The reaction solution was added to water and extracted with ethyl acetate. The aqueous layer was acidified by using 1 N aqueous solution of hydrochloric acid, extracted with ethyl acetate, washed with saturated brine and dried over sodium sulfate. The drying agent was removed by filtration and the residues obtained after concentration under reduced pressure were purified by silica gel column chromatography (ethyl acetate/hexane) to obtain the target compound (white solid, 1.10 g, 84%).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US09440922B2uspto-grants-2016_09