反应详情

A solution of sulfuryl chloride (12.4 mmol) in toluene (5 mL) was added dropwise via an additional funnel to a solution of ethyl benzoylacetate (12.4 mmol) in toluene (20 mL) over 5 minutes at room temperature. The resulting mixture was stirred at room temperature overnight. Water was added slowly and resulting two-phase mixture was basified with saturated NaHCO3 and extracted with ethyl acetate. The combined organic extracts were washed with brine, dried over anhydrous sodium sulfate, and evaporated to afford 2.2 g (84%) of product as a pale yellow oil; MH+=227.0, retention time (LC-MS)=2.77 min.

1. customresulting two-phase mixture
2. extractionextracted with ethyl acetate
3. washThe combined organic extracts were washed with brine
4. dry with materialdried over anhydrous sodium sulfate
5. customevaporated