An Isolable Radical Anion Based on the Borole Framework
An Isolable Radical Anion Based on the Borole Framework
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DOI：
10.1002/anie.201108632
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发表时间：
2012-01-01
影响因子：
16.6
通讯作者：
Wahler, Johannes
中科院分区：
文献类型：
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作者：
Braunschweig, Holger;Dyakonov, Vladimir;Wahler, Johannes
方法A：将(5)（101 mg, 251 μmol）与甲西基锂（85.0 mg, 674 μmol）的混合物冷却至10℃，加入苯（1.5 mL）。将混合物在室温下搅拌19小时，形成深绿色溶液和无色沉淀物。过滤后将溶液浓缩得到[MesBC4Ph4 (C6H6)](4)的墨绿色晶体。用注射器除去溶液，用正己烷（0.2 mL）洗涤结晶，真空干燥得到[MesBC4Ph4 (C6H6)](4)(58.0 mg, 103 μmol, 41%)，为深绿色结晶。以苯/己烷为原料，通过重结晶得到了适合x射线衍射的单晶。
Method A: A mixture of (5)(101 mg, 251 μmol) and mesityllithium (85.0 mg, 674 μmol) was cooled to 10 C and benzene (1.5 mL) was added. The mixture was stirred at ambient temperature for 19 h resulting in formation of a dark green solution and a colorless precipitate. After filtration, the solution was concentrated to give dark green crystals of [MesBC4Ph4 (C6H6)](4). The solution was removed via syringe, the crystals were washed with hexane (0.2 mL) and dried under vacuum to yield [MesBC4Ph4 (C6H6)](4)(58.0 mg, 103 μmol, 41%) as a dark green, crystalline solid. Single crystals suitable for X-ray diffraction were obtained by recrystallization from benzene/hexane.