反应详情

m-Bromotoluene (34.2 g) in dry ether (120 ml) was added dropwise to magnesium turnings (4.8 g) in dry ether (100 ml). The heat of reaction maintained the mixture to boiling under reflux during the addition and the mixture was heated under reflux for a further hour. The mixture was cooled to 0°, dry cadmium chloride (19.6 g) was added and the temperature allowed to rise to 20° C. After 1 hour, cyclopropanecarbonyl chloride (20.8 g) in dry ether (50 ml) was added dropwise and the mixture was heated under reflux for 4 hours, cooled to 0° and treated with 2 N hydrochloric acid. The ether layer was separated, washed with aqueous sodium bicarbonate (3× 100 ml., 8%) and with water, dried over magnesium sulphate, filtered and evaporated. The residue was distilled under reduced pressure and the fraction b.p. 86°-90°/0.4 mm was collected.

1. temperatureThe heat of reaction
2. temperaturemaintained the mixture
3. temperatureunder reflux during the addition
4. temperaturethe mixture was heated
5. temperatureunder reflux for a further hour
6. temperatureThe mixture was cooled to 0°
7. customto rise to 20° C
8. temperaturethe mixture was heated
9. temperatureunder reflux for 4 hours
10. temperaturecooled to 0°
11. customThe ether layer was separated
12. washwashed with aqueous sodium bicarbonate (3× 100 ml., 8%) and with water
13. dry with materialdried over magnesium sulphate
14. filtrationfiltered
15. customevaporated
16. distillationThe residue was distilled under reduced pressure
17. customthe fraction b.p. 86°-90°/0.4 mm was collected