反应详情

温度

100 °C

To a solution of ethyl 5-bromo-2-chlorobenzoate (1.9 g) in DMF (12 mL), toluene (0.3 mL), cyclopropylacetylene (714 mg), copper iodide (275 mg), dichloro bis(triphenylphosphine)palladium (1.01 g) and triethylamine (20.1 mL) were added, and the mixture was degassed, stirred at 100° C. under argon atmosphere for 8 hours, and then the reaction mixture was cooled to room temperature and diluted with ethyl acetate. The insoluble material was filtered off on celite. The mother liquor was washed with brine, dried over magnesium sulfate and concentrated. By purification on column chromatography, ethyl 2-chloro-5-(cyclopropylethynyl)benzoate (1.86 g) was obtained as brown oil.

1. customthe mixture was degassed
2. temperaturethe reaction mixture was cooled to room temperature
3. additiondiluted with ethyl acetate
4. filtrationThe insoluble material was filtered off on celite
5. washThe mother liquor was washed with brine
6. dry with materialdried over magnesium sulfate
7. concentrationconcentrated
8. customBy purification on column chromatography