反应详情

A solution of norbornylfulvene (14.37 g, 90.8 mmol) dissolved in 100 mL tetrahydrofuran was cooled to 0° C. before LiAlH4 (5.00 g, 132 mmol) was added over 2 minutes. After stirring at room temperature for 17 hours, the reaction was cooled to 0° C. and 100 mL water were added dropwise over 1 hour. Then, 200 mL water/50 mL concentrated aqueous HCl and 100 mL diethyl ether were added. The organic layer was isolated and the aqueous layer was extracted with diethyl ether (3×50 mL). The organic layers were dried over MgSO4, filtered, and rotavapped to provide the crude product as a light yellow oil in quantitative yield.

1. additionwas added over 2 minutes
2. temperaturethe reaction was cooled to 0° C.
3. customThe organic layer was isolated
4. extractionthe aqueous layer was extracted with diethyl ether (3×50 mL)
5. dry with materialThe organic layers were dried over MgSO4
6. filtrationfiltered