问题：求一化合物的合成方法
类型：求助 (悬赏分:3分)
提问：lin3ye
等级：▲
版块：文献检索技术、各类代理(wguoyong,wangjinyon,)
信誉：79%
回复：1
阅读：785
时间：2011-04-14 10:22:59 编辑加入/取消收藏订制/取消短消息举报该贴

化合物名称： 4,4’-bis(dimethylsilyl)-biphenyl
CAS 号：暂无
求合成方法！！scifinder 贝尔斯坦均可

回复人：tangyyer,★★★★★ (有空来逛逛my blog: http://tangyyer.blog.hexun.com) 时间：2011-04-18 09:15:42 编辑

1楼

Preparation of 4,4'-Bis(dimethylsilyl)biphenyl. To a
solution of 64.1 mmol of 4,4'-biphenylylenedimagnesium di-
bromide prepared from 1.56 g of magnesium and 20.0 g of 44'-
dibromobiphenyl in 50 mL of THF was added dropweise 13
mL of chlorodimethylsilane at 0 "C. The resulting mixture
was stirred overnight at room temperature, and then hydro-
lyzed with water. The organic layer was separated, and the
aqueous layer was extracted with chloroform. The organic
layer and extracts were combined, washed with water, and
then dried over anhydrous magnesium sulfate. After the
solvent was evaporated, the residue was distilled under
reduced pressure to give 8.0 g (46% yield) of 4,4'-bis-
(dimethylsily1)biphenyl: bp 106 "C (1 mmHg); MS mlz 270
(M+); IH NMR (6 in CDCl3) 0.42 (d, 12H, J = 3.6 Hz, MeSi),
4.52 (sept, 2H, J = 3.6 Hz, HSi), 7.64 (d, 4H, J = 8.6 Hz, ring
protons), 7.67 (d, 4H, J = 8.6 Hz, ring protons); 13C NMR (6
in CDC13) -3.7, 126.6, 134.5, 136.4, 141.8. Anal. Calcd for
Cld-hSiz: C, 71.04; H, 8.20. Found: C, 70.98; H, 8.00.

问题讨论没有结束...

您尚未进入本论坛,登录之后才可以回贴

5msec