反応 #46169

ord-23c10cc71dab4da2b36ff644b173985a

反応条件

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

後処理

  1. 1
    抽出Then, the mixture was extracted with ethyl acetate/saturated sodium chloride
  2. 2
    乾燥The extract was dried over anhydrous magnesium sulfate
  3. 3
    濃縮concentrated
  4. 4
    その他the resulting residue was purified by column chromatography

実験手順

Sodium hydride (3.1 g, 77.1 mmol) and diethyl carbonate were combined with 3-methylacetophenone (4.5 g, 33.54 mmol). The mixture was stirred for 2 hours at 80° C. After the reaction was completed, ice water and acetic acid were added thereto. Then, the mixture was extracted with ethyl acetate/saturated sodium chloride. The extract was dried over anhydrous magnesium sulfate, concentrated, and the resulting residue was purified by column chromatography to obtain 3-oxo-3-m-tolylpropionate ethyl ester (5.8 g, yield 84%).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07741323B2uspto-grants-2010_06