反应详情

温度

120 °C

A mixture of diethyl 2-(4-bromo-2-methoxyphenyl)malonate (1213 mg, 3.500 mmol), lithium chloride (620 mg, 14.6 mmol), and DMSO (6 ml) was stirred at 120° C. for 20 hours, then at 150° C. for 4 hours, and again at 120° C. for 20 hours. The reaction was cooled to room temperature, diluted with 25 mL of water, and extracted with ethyl acetate-heptane mixture (1:1). The extract was washed with brine (2 times), dried over magnesium sulfate, and loaded on silica gel. Chromatography on a silica gel column, eluting with a gradient from 0% to 30% of ethyl acetate in heptane gave the title compound (405 mg, 42% yield over two steps). GCMS (ES+) 272 (M+).

1. waitat 150° C. for 4 hours
2. waitagain at 120° C. for 20 hours
3. temperatureThe reaction was cooled to room temperature
4. extractionextracted with ethyl acetate-heptane mixture (1:1)
5. washThe extract was washed with brine (2 times)
6. dry with materialdried over magnesium sulfate
7. washChromatography on a silica gel column, eluting with a gradient from 0% to 30% of ethyl acetate in heptane