反应详情

For example, magnesium turnings (6.4 g, 0.26 mole) were flame-dried, the containing glassware was cooled, and 3-bromochlorobenzene (50 g, 0.26 mole), in 50 ml of diethyl ether was added. As the reaction began, an additional 200 ml of diethyl ether was added, and the reaction mixture was heated under reflux for 0.5 hour. To the refluxing reaction mixture was added dropwise, during a 0.5 hour period, 3-methylcyclohexanone (29.2 g, 0.26 mole) in 100 ml of diethyl ether. Upon complete addition, the reaction mixture was heated under reflux for an additional 0.5 hour, then poured into 500 ml of icewater containing 50 ml of hydrochloric acid. The mixture was extracted with three 200 ml portions of diethyl ether. The combined extract was washed twice with 100 ml portions of an aqueous solution saturated with sodium chloride. After separation, the organic layer was dried over sodium sulfate and filtered. The filtrate was evaporated under reduced pressure to an oil. The oil was purified by distillation using a Kugelrohr distilling system at 85°/0.05 mm for 2.5 hours to give 1-(3-chlorophenyl)-3-methylcyclohexan-1-ol (25 g).

1. temperaturethe containing glassware was cooled
2. temperaturethe reaction mixture was heated
3. temperatureunder reflux for 0.5 hour
4. customTo the refluxing reaction mixture
5. additionwas added dropwise, during a 0.5 hour period
6. additionUpon complete addition
7. temperaturethe reaction mixture was heated
8. temperatureunder reflux for an additional 0.5 hour
9. additionpoured into 500 ml of icewater
10. extractionThe mixture was extracted with three 200 ml portions of diethyl ether
11. extractionThe combined extract
12. washwas washed twice with 100 ml portions of an aqueous solution saturated with sodium chloride
13. customAfter separation
14. dry with materialthe organic layer was dried over sodium sulfate
15. filtrationfiltered
16. customThe filtrate was evaporated under reduced pressure to an oil
17. distillationThe oil was purified by distillation
18. distillationdistilling system at 85°/0.05 mm for 2.5 hours