反応 #505943

ord-0c1f8af702904fe2aba272a33a724426

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.STIRRINGAfter stirring at room temperature for 20 h
  2. 2
    その他to separate the phases
  3. 3
    抽出The aqueous layer was extracted again with toluene
  4. 4
    濃縮the combined organic layer was concentrated under reduced pressure
  5. 5
    その他the residue thus obtained

実験手順

To a solution of 2-(4-hydroxybenzyl)-3-isopropylmaleic acid dimethyl ester (44.1 mg, 0.151 mmol) in (880 μL) were added potassium carbonate (34.7 mg, 0.251 mmol) and methyl bromoacetate (138.4 mg, 0.904 mmol) with stirring at room temperature. After stirring at room temperature for 20 h, the reaction mixture was diluted with toluene and water to separate the phases. The aqueous layer was extracted again with toluene, and the combined organic layer was concentrated under reduced pressure and the residue thus obtained was subjected to silica gel column chromatography (toluene-ethyl acetate 10:1) to give 45.2 mg of the title compound as oil (yield: 82%).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08093294B2uspto-grants-2012_01