High-selectivity silane-based olefin and preparation method thereof
An alkyl olefin, high-selectivity technology, applied in chemical instruments and methods, silicon-organic compounds, organic chemistry, etc., can solve the problems of low regional and stereoselectivity, difficult conversion, etc., and achieve low regional and stereoselectivity. , to solve the transformation difficulties, the effect of mild reaction conditions
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Embodiment 1
[0033] A kind of preparation method of highly selective gem-disilazyl olefin comprises the following steps:
[0034](1) Weigh 0.02mmol iron triacetylacetonate, 0.04mmol 1,3-bis(diphenylphosphine)propane and 0.55mmol sodium tert-butoxide in a glove box and put them into a pressure-resistant sealed tube to obtain mixed raw materials, take out After connecting the double-row pipe, use nitrogen to pump and ventilate 3 times, each time at an interval of 4 minutes, and then replace the rubber plug and then use nitrogen to pump and ventilate 3 times, each time at an interval of 4 minutes;
[0035] (2) Add 0.2mmol (5,5-difluoropent-4-en-1-yl)benzene, 0.7mmol triethyl (4,4,5, 5-Tetramethyl-1,3,2-dioxaborolan-2-yl)silane and 1mL tetrahydrofuran were reacted at 70°C and 520rpm for 12h to obtain the reactant;
[0036] (3) Quench the reactant obtained in step (2) with a saturated solution of ammonium chloride, then extract 3 times with ethyl acetate, 30 mL each time, combine the organic p...
Embodiment 2
[0042] A preparation method of highly selective Z-fluorosilyl olefins, comprising the following steps:
[0043] (1) Take by weighing 0.02mmol ferrous iodide, 0.02mmol 1,3-bis(diphenylphosphine)butane and 0.9mmol sodium tert-butoxide in a glove box and put it into a pressure-resistant sealed tube to obtain the mixed raw materials, After taking it out, connect the double-row pipe with nitrogen pumping for 3 times, each interval of 4 minutes, and then replace the rubber plug and then use nitrogen pumping for 3 times, each interval of 4 minutes;
[0044] (2) Add 0.2mmol (4,4-difluorobut-3-en-1-yl)benzene, 0.5mmol triethyl (4,4,5, 5-Tetramethyl-1,3,2-dioxaborolan-2-yl)silane and 1mL tetrahydrofuran were reacted at -20°C and 450rpm for 12h to obtain the reactant;
[0045] (3) Quench the reactant obtained in step (2) with a saturated solution of ammonium chloride, then extract 3 times with ethyl acetate, 30 mL each time, combine the organic phases, dry over anhydrous sodium sulfate,...
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