반응 #46158

반응 방정식

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

수율 76.5%

용매

Dimethylformamide

반응 조건

후처리

1. 1
   추출The reaction mixture was extracted with ammonium chloride and ether
2. 2
   기타the organic layer was separated
3. 3
   건조dried over anhydrous magnesium sulfate
4. 4
   농축concentrated
5. 5
   기타the resulting residue was purified by column chromatography

실험 절차

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%).

출처