摘要
1,3-二氯四甲基二硅氧烷相继与环戊二烯基钠、钠砂及 MCl_4反应,制得标题化合物:O(SiMe_2)_2(C_5H_4)_2MCl_2(1,M=Ti;2,M=Zr;3,M=Hf).考察了1的卤素置换反应:1与(NH_4)_2SiF_6作用生成相应的二氟化物4,4与氢溴酸作用生成相应的二溴化物5.经元素分析,UV,~1H(^(13)C)NMR 和 MS 表征了它们的结构,并利用 X 射线衍射法测定了2和3的晶体和分子结构.化合物1,2和3的有关结构数据比较表明,由于中心金属的不同而引起其键长和键角的差异与其碳桥类似物(CH_2)_3(C_5H_4)_2MCl_2的情况相似.
The title compounds O(Me_2Si)_2(C_5H_4)_2MCl_2(1,M=Ti;2,M=Zr;3,M=Hf) weresynthesized by the reaction of 1,3-dichlorotetramethyl disiloxane with cyclo-penta-dienyl sodium,followed with sodium sands and then with MCl_4.The halogen exchangereaction of 1 was examined.Reaction of 1 with (NH_4)_2SiF_6 yields the correspondingdiflouride 4,and reaction of 4 with hydrobromic acid yields the correspondingdibromide 5.They were characterized by elemental analysis,UV,~1H NMR,^(13)C NMRand MS.The structures of 2 and 3 were confirmed by X-ray structure analysis.Relevant data comparison of 1,2 and 3 showed that the difference of the bonddistances and bond angles due to different central metal atom is similar to the carbo-bridged analogues (CH_2)_3(C_5H_4)_2MCl_2.
出处
《化学学报》
SCIE
CAS
CSCD
北大核心
1991年第11期1107-1113,共7页
Acta Chimica Sinica