反应详情

温度

105 °C

A mixture of 2-benzylmalonic acid (10.0 g, 51.5 mmol), 2,4,6-trichlorophenol (20.3 g, 103 mmol), and POCl3 (12.0 mL, 129 mmol) was stirred under air at 105° C. for 2 hours. The reaction was then cooled to room temperature, poured on 150 mL ice, and extracted with 4:1 ether/DCM (3×150 mL). The combined organic layers were washed with water (1×400 mL) and 4 M aqueous NaCl (1×100 mL), and the yellow organic layer was dried (Na2SO4), filtered, and concentrated by rotary evaporation at <40° C. to provide the title compound as a tan thick oil that became a beige solid upon standing.

1. temperatureThe reaction was then cooled to room temperature
2. extractionextracted with 4:1 ether/DCM (3×150 mL)
3. washThe combined organic layers were washed with water (1×400 mL) and 4 M aqueous NaCl (1×100 mL)
4. dry with materialthe yellow organic layer was dried (Na2SO4)
5. filtrationfiltered
6. concentrationconcentrated by rotary evaporation at <40° C.