反応 #46158

反応方程式

5-Chloromethyl benzo[1,3]dioxol

potassium carbonate

sodium iodide

ethyl benzoylacetate

→

2-benzo[1,3]dioxol-5-ylmethyl-3-oxo-3-phenylpropionate ethyl ester

収率 76.5%

溶媒

Dimethylformamide

反応条件

後処理

1. 1
   抽出The reaction mixture was extracted with ammonium chloride and ether
2. 2
   その他the organic layer was separated
3. 3
   乾燥dried over anhydrous magnesium sulfate
4. 4
   濃縮concentrated
5. 5
   その他the resulting residue was purified by column chromatography

実験手順

5-Chloromethyl benzo[1,3]dioxol (11.2 g, 65.7 mmol) was dissolved in Dimethylformamide. Then, potassium carbonate (18.2 g, 131.4 mmol), sodium iodide (10.8 g, 72.27 mmol) and ethyl benzoylacetate (12.5 ml, 72.27 mmol) were added thereto and stirred for 5 hours at room temperature. The reaction mixture was extracted with ammonium chloride and ether, the organic layer was separated, dried over anhydrous magnesium sulfate, concentrated, and the resulting residue was purified by column chromatography to obtain 2-benzo[1,3]dioxol-5-ylmethyl-3-oxo-3-phenylpropionate ethyl ester (16.4 g, 76%).

出典