Siloxanes and silylamines with fluoromethyl-methylsilicon groups: X-ray study of [CH2F(CH3)SiO]4
作者:Helmut Beckers、David J. Brauer、Hans Bürger、Ralf Gielen、Peter Moritz
DOI:10.1016/0022-328x(95)05931-e
日期:1996.4
CH2FMe2SiBr (II) was prepared by the reaction of CH2FMe2SiH with Br2. The solvolysis of II with H2O and NH3 gave (CH2FMe2Si)2O (III) and (CH2FMe2Si)2NH (IV) respectively. After lithiation with n-BuLi and thereafter reaction with II, compound IV afforded the trisilylamine (CH2FMe2Si)3N (V). Hydrolysis of CH2FMeSiBr2 (I) with H2O yielded a polysiloxane oil from which 10% of a crystalline material (VI)
CH 2 FME 2 SIBR(II)是由CH的反应而制备2 FME 2的SiH被Br 2。II用H 2 O和NH 3溶剂分解分别得到(CH 2 FMe 2 Si)2 O(III)和(CH 2 FMe 2 Si)2 NH(IV)。用正丁基锂锂化,然后与II反应后,化合物IV得到三甲硅烷基胺(CH 2 FMe 2Si)3 N(V)。CH 2 FMeSiBr 2(I)与H 2 O的水解产生聚硅氧烷油,从其中分离出10%的结晶材料(VI)。通过分析,质量,NMR和IR光谱表明这是环四硅氧烷(CH 2 FMeSiO)4。NMR光谱表明所有可能的立体异构体都是随机分布的。VI的单晶通过X射线衍射检查。基本平面的Si 4 O 4找到了环,SiOSi角平均为157.9(5)°。由于F原子无序性很大,因此在环境温度下的填充要求而非晶体的固有构象含量可能会施加于环上的晶体学反演对称性。