A kind of silane compound and its preparation method and application
A technology for silane compounds and hexasilane, which is applied in the fields of silane compounds and their preparation and application, can solve problems such as complicated preparation process, and achieve the effects of high activity, high isotacticity and wide molecular weight distribution.
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Embodiment 1
[0030] In a reaction flask, under nitrogen protection and anhydrous conditions, add 9,9-dimethylolfluorene (5.7 g), triethylamine (5 ml) and tetrahydrofuran (80 ml), and cool in an ice-water bath for 1 hour A mixed solution of diallyldichlorosilane (2.3 g) and tetrahydrofuran (40 ml) was added dropwise. After the addition, the mixture was reacted at room temperature for 12 hours, and heated under reflux for 3 hours. Then add saturated aqueous ammonium chloride solution, stir, and separate the organic phase. Extracted three times with ether, and combined the organic phases. After washing with water and a saturated sodium chloride solution successively, and drying over anhydrous sodium sulfate, the solvent was distilled off under reduced pressure. The residue was separated and purified by column chromatography to obtain 1.7 g of product 2,2-diallyl-5,6,7,8-dibenzo-1,3,2-dioxaspirosilane. 1 H-NMR (δ, ppm, TMS, CDCl 3 ): 7.25~8.17 (8H, m, ArH), 5.73 (2H, m, =CH), 5.02 (4H, m, =...
Embodiment 2
[0032] In a reaction flask, under nitrogen protection and anhydrous conditions, add 2,4-pentanediol (5.2 grams), triethylamine (10ml) and tetrahydrofuran (100ml), under the cooling condition of 0 ~ 10 ℃ in A mixed solution of diallyldichlorosilane (4.6 g) and tetrahydrofuran (40 ml) was added dropwise within 1 hour. After the addition was complete, the mixture was reacted at room temperature for 12 hours and then heated under reflux for 8 hours. After the temperature dropped to room temperature, a saturated ammonium chloride aqueous solution was added, stirred, and the organic phase was separated. Extracted three times with ether, and combined the organic phases. It was washed with water and saturated sodium chloride solution successively, dried over anhydrous sodium sulfate, and the low boiling point solvent was distilled off under reduced pressure. The residue was separated and purified by column chromatography to obtain 2.6 g of the product 2,2-diallyl-4,6-dimethyl-1,3,2-d...
Embodiment 3
[0034] In a reaction flask, under nitrogen protection and anhydrous conditions, 3-methyl-2,4-pentanediol (3.2 g) and anhydrous ether (80 ml) were added dropwise to diallyl dichlorosilane ( 2.0 g) and tetrahydrofuran (40ml) mixed solution, after stirring and dissolving, add potassium tert-butoxide (0.02mol) in batches within 1 hour, keep room temperature reaction for 8 hours after adding, then heat and reflux for 4 hours, cool to room temperature. The extracted solution was washed three times with anhydrous ether, the organic phases were combined, washed thoroughly with saturated sodium chloride, dried with anhydrous sodium sulfate, and the low boiling point solvent was distilled off under reduced pressure. The residue was separated and purified by column chromatography to obtain 1.2 g of the product 2,2-diallyl-5-ethyl-4,6-dimethyl-1,3,2-dioxacyclohexasilane. 1 H-NMR (δ, ppm, TMS, CDCl 3 ): 5.72(2H,m,=CH), 5.00(4H,m,=CH 2 ), 3.40 (2H, s, OCH), 1.54~1.78 (5H, m, CH and SiCH ...
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