反应详情

To a single-neck reaction flask (250 mL) were added (E)-trimethylsilyl 2-butenoate (12.242 g, 77.481 mmol), NBS (16.550 g, 92.977 mmol), (PhCO2)2 (310 mg) and carbon tetrachloride (100 mL). The mixture was stirred under reflux for 3.5 hr. The resulting mixture was cooled in an ice-water bath. The insoluble substance was filtered. The residue was rotatory-evaporated and concentrated until no liquid dropped. The concentrate was distilled under reduced pressure to collect the fraction under 9 mmHg at the temperature of 100° C.-102° C. to give the target compound as a colorless transparent liquid.

1. temperatureunder reflux for 3.5 hr
2. temperatureThe resulting mixture was cooled in an ice-water bath
3. filtrationThe insoluble substance was filtered
4. customThe residue was rotatory-evaporated
5. concentrationconcentrated until no liquid
6. additiondropped
7. distillationThe concentrate was distilled under reduced pressure
8. customto collect the fraction under 9 mmHg at the temperature of 100° C.-102° C.