(Dimethoxymethylsilyl)benzene

Colorless or yellowish transparent liquid

Liquid

The methylphenyldichlorosilane and the hydrogen chloride absorber anhydrous calcium carbonate were added to the alcohol to be stirred and stirred in a molar ratio of 1: 2, and the catalyst sodium methoxide was added to the anhydrous methanol to dissolve to obtain an anhydrous sodium methoxide solution , Control the catalyst sodium methoxide and anhydrous methanol molar ratio of 1:10 and then take the air, nitrogen replacement, and then constant pressure slowly to the reactor by adding anhydrous sodium methoxide methanol solution, control methyl phenyl dichlorosilane and The molar ratio of anhydrous sodium methoxide methanol solution was 1: 2, the dropping time was 1h, the reaction temperature was 40 , and the reaction was completed at 70 for 1h. After the reaction was complete, the reaction was carried out to obtain methylphenyldi Methoxysilane. (2) adding crude methylphenyldimethoxysilaneTo homemade gradient efficient distillation tower kettle, Control distillation temperature 64 ~ 65 fractionation recovery of methanol, And then controlled by adjusting the reflux ratio of 199 ~ 200 Distillation of high content of more than 99.5percent of high-quality methylphenyldimethoxysilane, Product quality reached the international advanced level; (3) passing the hydrogen chloride gas generated in the alcoholysisFalling film absorption system is recycled to produce more than 25percent hydrochloric acid for sale.The whole system through 2L / min nitrogen, Wherein the whole system comprises 88.6percent of the yield of methylphenyldimethoxysilane obtained by the alcoholysis of the closed stirring reaction system and the distillation system, Colorless transparent liquid, Relative density 1.006g / m (20 ), boiling point 199 ~ 201 , refractive index 1.481, Flash point (open cup) 80 , methylphenyldimethoxysilane content of 99.51percent, high boiling content of 0. 1percent.Sodium metal particles suspension was added to a mixture of 62.5 g of chlorobenzene and 227 g of methyltrimethoxysilane, and then 0.32 g of 15-crown-5 was added. The reaction was carried out at 38 ° C for 2 h , The reaction was stopped, and the reaction mixture was filtered and vacuum-distilled to give methylphenyldimethoxysilane in a yield of 87percent.Into a four-necked flask, 12 g of magnesium powder (0.5mol), 18 g of tetrahydrofuran (0.25mol), methyltrimethoxysilane 9.5G (0.07mol), chlorobenzene 3.4 g (0.03mol); was stirred and heated to reflux to start the reaction. Under reflux for about 1 hourSolution containing 90.1 g (0.8mol) of chlorobenzene, 29.9 g (0.2mol) methyl trichlorosilane and 177 g (1.3mol) methyltrimethoxysilane A mixed solution of methoxysilane; refluxing continued for 6.5h; cooled to room temperature, suction filtered, washed with an appropriate amount of methyltrimethoxysilane cakeTwice the combined filtrate is the crude product. By gas chromatographic analysis, the yield of methyl phenyl dimethoxysilane was 85.5percent (magnesiumCalculation). The crude product was distilled at atmospheric pressure to recover unreacted material, a vacuum distillation to give the product methylphenyl dimethoxysilane, purity99.6percent.A suspension of sodium metal particles was added to a mixture of 87. 22 g of bromobenzene and 227 g of methyltrimethoxysilane, Then added0.32 g of cyclodextrin, The reaction was stopped at 38 ° C for 2 h, and the reaction mixture was filtered and reduced in vacuum to give methylphenyldimethoxysilane in a yield of 80percent.5L four-necked flask by adding 240g methyltrimethoxysilane and 1000mL ether, stirring drop 1080mL 1.63mol / L bromobenzene reagent ether solution; drop Bi, heated reflux 1h .; cooling, to the reaction (Yield 95percent) of phenylmethyldimethoxysilane and 4 g of diphenylmethoxysilane (yield 1percent) were added to the filtrate by adding 1000 mL of n-hexane and then filtering.(This example, as a comparative example, does not include the addition of 241 g of methyltrimethoxysilane and 1000 mL of tetrahydrofuran in a 5 L four-necked bottle within the scope of the present invention, starting with stirring, dropping 1030 mL of 1.72 mol / L Chlorophenyl Grignard reagent in tetrahydrofuran After 1 hour of reaction, most of the tetrahydrofuran was distilled off and 1000 mL of xylene was added and the remaining tetrahydrofuran was distilled off and allowed to cool to room temperature and filtered to give 99 g of phenylmethyldi Methoxysilane (yield 31percent) and 69 g of diphenylmethylmethoxysilane (yield 17percent).General procedure: A mixtureof methanol (2 mL), distilled water (0.09 g, 5 mmol), and trimethylchlorosilane(0.01 g) was slowly added dropwise to a vigorosuly stirred solution of the appropriate silane (0.01 mol) in methanol (10 mL). Trimethylchlorosilane was used as a sourceof hydrogen chloride. The reaction mixture was stirred for 10 hand allowed to stand for 16 h. Excess methanol was removedin vacuo. Compound 1 (59%) was isolated by distillation; compound2 (67%), by recrystallization from pentane.1, 3-Dimethoxy-1, 3-dimethyl-1, 3-diphenyldisiloxane (1). B.p.155-158 C (5 Torr). 1H NMR, : 0.26 (s, 6 H, Me-Si); 3.36(s, 6 H, MeO); 7.23-7.43 (m, 10 H, Ph). 13C NMR, delta: -2.92(Me-Si); 50.06 (MeO); 127. 57, 129.74, 133.36, 134.90 (Ph).29Si NMR, delta: -23.22. IR (fi lm), /cm-1: 481; 584; 706, 733, 783, 808, 1081; 1116; 1311; 1427; 1461; 1591; 1772; 1826; 1895;1962; 2836; 2968; 3011; 3059. Found (%): C, 59.58; H, 6.92.C16H22O3Si2. Calculated (%): C, 60.33; H, 6.96.

Intermediates

Molecular Weight:182.29
Hydrogen Bond Acceptor Count:2
Rotatable Bond Count:3
Exact Mass:182.076306220
Monoisotopic Mass:182.076306220
Topological Polar Surface Area:18.5
Heavy Atom Count:12
Complexity:129
Covalently-Bonded Unit Count:1
Compound Is Canonicalized:Yes