- cis-trans-cis-Tetrabromotetramethylcyclotetrasiloxane: A versatile precursor of ladder silsesquioxanes
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The title compound was isolated for the first time by a novel procedure including dephenylbromination of cyclotetrasiloxane. The stereostructure of the tetrabromide was confirmed by condensation with diphenylsilanediol, affording anti-tricyclo[7.3.1.13.7]hexasiloxane. This tetrabromide spontaneously decomposed in air to afford a white powder insoluble in organic solvents. Measurements of the TG, IR, and solid-state NMR spectra of the product revealed that a ladder polysilsesquioxane with high thermal stability and stereoregularity was obtained.
- Unno, Masafumi,Chang, Shengho,Matsumoto, Hideyuki
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- A functionality do not contain impurity methyl phenyl cyclosiloxane method for the preparation of
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The invention relates to a preparation method of methylphenyl cyclosiloxane without containing polyfunctional impurities. The preparation method comprises the following steps: (A) sequentially adding a polar aprotic solvent, methylphenyl dialkoxysilane, water and a catalyst into a reactor for hydrolysis and condensation reaction, distilling out alcohol and water, and when the refractive index nD25 of distillate is nearly 1.3325, stopping the reaction; (2) gradually heating to 110-160 DEG C, and cracking the catalyst in a refluxing state; (3) after cracking the catalyst, distilling out and recycling the solvent, wherein an undistilled part in the reactor is a crude product; (4) distilling and purifying the crude product, and collecting methylphenyl cyclosiloxane distillate, namely obtaining a finished product. In the whole process, organic acid, inorganic acid or an alkali metal hydroxide is not used as a catalyst, and complex operations, such as neutralizing, water washing, filtering and the like rare not required; the reaction is easy to control; the yield of the finished product is as high as 90.0-97.1%; the purity of the finished product is 98.1-99.99%.
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Paragraph 0048; 0049; 0054
(2017/04/29)
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