Gem-disilicon compound as well as preparation method and application thereof
A silicon compound and reaction technology, applied in the field of new gem-disilicon compounds, can solve problems such as unsatisfactory regioselectivity, single structure type, and limited synthesis methods
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Embodiment 1
[0073] Example 1: Preparation of gem-disilicon compounds by iron-catalyzed hydrosilation of alkynes
[0074]
[0075] Weigh 2,9-di-2,4,6-triethylbenzene-1,10-phenanthroline ferrous chloride C1a (10.9mg, 0.017mmol, 5mol%) into a 10mL sealed tube in the glove box , Pour 1 mL of tetrahydrofuran (THF) into the reaction tube, and stir evenly to obtain an orange-yellow clear liquid. Add 42 μL of ethylmagnesium bromide (EtMgBr, 1M in Hexane, 12mol%) to activate the system, and react for 2 minutes to obtain a brown-black clear solution. Add phenylsilane (PhSiH 3 , 82.5mg, 0.76mmol, 2.2equiv), alkyne 1a (50mg, 0.35mmol, 1equiv), stir well. Seal the reaction tube, react at 30°C for 6h, and monitor the end of the reaction by NMR. Add n-pentane to the system, transfer the reaction solution to a round bottom bottle, and remove the solvent under reduced pressure. The residue was subjected to silica gel column chromatography (n-pentane as the eluent) to obtain 115 mg of colorless liqu...
Embodiment 2
[0131] Example 2: Iron Catalyst Evaluation Experiment for Alkyne Doublesilylation Reaction
[0132]
[0133] Weigh iron catalysts C1-C3 (0.017mmol, 5mol%) into a 10mL sealed tube in a glove box, inject 1mL tetrahydrofuran (THF) into the reaction tube, and stir evenly. Add 42 μL of ethylmagnesium bromide (EtMgBr, 1M in THF, 12mol%) to activate the system, and react for 2 minutes to obtain a brown-black clear solution. Add phenylsilane (PhSiH 3 , 82.5 mg, 0.76mmol, 2.2equiv), alkyne 1a (50mg, 0.35mmol, 1equiv), stir well. Seal the reaction tube, react at 30°C for 6h, and monitor the end of the reaction by NMR. Add n-pentane to the system, transfer the reaction solution to a round bottom bottle, and remove the solvent under reduced pressure. After the residue was subjected to silica gel column chromatography (with n-pentane as eluent), mes-trimethoxybenzene was added as an internal standard, and the yield of each product was determined by NMR. The obtained experimental res...
Embodiment 3
[0136] Example 3: Additive evaluation experiment for alkyne double silylation reaction
[0137]
[0138] Weigh 2,9-di-2,4,6-triethylbenzene-1,10-phenanthroline ferrous chloride C1a (10.9mg, 0.017mmol, 5mol%) into a 10mL sealed tube in the glove box , Pour 1 mL of tetrahydrofuran (THF) into the reaction tube, and stir evenly to obtain an orange-yellow clear liquid. Add additives (12mol%), after reacting for 2min, add phenylsilane (PhSiH 3 , 82.5mg, 0.76mmol, 2.2equiv), alkyne 1a (50mg, 0.35mmol, 1equiv), stir well. Seal the reaction tube, react at 30°C for 6 h, and monitor the end of the reaction by NMR. Add n-pentane to the system, transfer the reaction solution to a round bottom bottle, and remove the solvent under reduced pressure. After the residue was subjected to silica gel column chromatography (using n-pentane as eluent), mes-trimethoxybenzene was added as an internal standard, and the yield of each product was determined by NMR. The obtained experimental results...
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