反应详情

温度

-78 °C

Preparation 1. A one-liter flask was charged with 2,7-di-tert-butylfluorene (50 g, 179.6 mmol) and a stir bar, capped with a rubber septum, and placed under a nitrogen atmosphere. Diethyl ether (about 300 mL) was added via a cannula, and the resulting mixture was cooled to −78° C. in a dry-ice bath. This mixture was stirred at this temperature as n-butyllithium (21.5 mL of 10 M in hexanes, 215 mmol) was added slowly via syringe. After the addition of n-butyllithium was complete, the reddish solution was slowly warmed to room temperature and stirred overnight (at least about 12 hours), to provide an ether solution of 2,7-di-tert-butylfluorenyl lithium.

1. customPreparation 1
2. customcapped with a rubber septum
3. additionwas added slowly via syringe
4. temperaturethe reddish solution was slowly warmed to room temperature