Multifunctional organosilicon compound and related methods, compounds, and compositions
An organosilicon compound and multifunctional technology, which is applied in the field of functionalized siloxane and multifunctional organosilicon compounds, can solve the problems of difficulty in synthesizing functional organosilicon compounds, limiting general applicability, yield and purity reduction, etc.
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Embodiment 1
[0330] Example 1: Condensation of trimethylchlorosilane with AMA-silanol .
[0331] A 40 mL vial equipped with a magnetic stir bar was charged with AMA-silanol (4.1193 g), THF (10 mL) and NEt 3 (2340 μL; 1.05 equiv) to form a mixture. A solution of trimethylchlorosilane (2000 μL; 1.05 equiv) in THF (4 mL) was slowly added to the mixture to obtain a reaction mixture which was stirred at room temperature overnight under nitrogen atmosphere. Hexane (20 mL) was then added to the reaction mixture, and the resulting mixture was filtered through a fine-grit funnel to remove salts. The filtrate was concentrated to strip THF and hexane, and additional salt precipitate was filtered from the concentrate with a 20 micron syringe filter. The remaining volatiles were removed to obtain the product ("monofunctional-AMA Si-Me compound"), which was then analyzed by NMR (recovery amount: 5.1 g; yield: 98%; purity: 95%).
Embodiment 2
[0332] Example 2: Preparation of bifunctional-AMA Si-H transformant
[0333] A 1000 mL three-necked flask was equipped with a nitrogen outlet and thermocouple, addition funnel and nitrogen inlet, and a mechanical stirrer with a Teflon stir bar. Fill the flask with MeHSiCl 2 (10.6 mL; 100 mmol) and diethyl ether (400 mL) to give a solution which was stirred and cooled to 0°C using an ice bath. The addition funnel was charged with AMA-silanol (55.22 g; 200 mmol) and pyridine (16.1 mL; 200 mmol), and the resulting mixture was added dropwise to the stirred flask over a period of about 15 minutes (about 5 mL / min). solution to obtain a reaction mixture. A white precipitate formed immediately after the addition. After the addition was complete, GCMS indicated about 97% conversion of the silanol and formation of condensation products. Precipitated salts were then removed by filtration, and the filter cake was washed with diethyl ether (ca. 100 mL). The combined organics were wa...
Embodiment 3
[0334] Example 3: Preparation of bifunctional-AMA Si-vinyl converters
[0335] A 100 mL three-necked flask was equipped with a magnetic stir bar, nitrogen outlet and thermocouple, addition funnel and nitrogen inlet. Fill the flask with MeViSiCl 2 (1.63 mL; 12.5 mmol) and toluene (50 mL) to obtain a mixture which was stirred and cooled to 0° C. using an ice bath. AMA-silanol (6.9 g; 25 mmol) and pyridine (2.2 mL; 27.5 mmol) were charged to the addition funnel and added dropwise to the stirred mixture in the flask over a period of about 15 minutes to obtain a reaction mixture. A white precipitate formed immediately after the addition. After the addition was complete, GCMS indicated about 90% conversion of the silanol and formation of condensation products. Then add the additional part of MeViSiCl 2 (0.16 mL) and pyridine (0.22 mL). The precipitate (salt) was then removed by filtration and the filter cake was washed with toluene. The combined organics were washed with HC...
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