2,7-Di-tert-butylfluorene → HCID 178506710、化合物
反応式
[C:1]([C:5]1[CH:17]=[CH:16][C:15]2[C:14]3[C:9](=[CH:10][C:11]([C:18]([CH3:21])([CH3:20])[CH3:19])=[CH:12][CH:13]=3)[CH2:8][C:7]=2[CH:6]=1)([CH3:4])([CH3:3])[CH3:2].C([Li:26])CCC>CCOCC>[C:1]([C:5]1[CH:17]=[CH:16][C:15]2[C:14]3[C:9](=[CH:10][C:11]([C:18]([CH3:21])([CH3:20])[CH3:19])=[CH:12][CH:13]=3)[CH2:8][C:7]=2[C:6]=1[Li:26])([CH3:4])([CH3:3])[CH3:2]参加物
4
反応条件
- 温度
- -78 °C
実験手順
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.