(1-(substituted phenyl)acenaphthylene)-bis(3,5-bis(trifluoromethyl))phenylphosphine compound and preparation method thereof
A technology of trifluoromethyl and phenylphosphine, which is applied in the field of organochemical metal-catalyzed ligand synthesis, can solve the problems of large influence on reaction activity, low yield of coupling products, weak conjugation effect, etc., and achieve a single product , Improve the coupling yield, and promote the effect of strong effect
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Embodiment 1
[0138] Preparation of (1-(phenyl)acenaphthenyl)-bis(3,5-bis(trifluoromethyl))phenylphosphine
[0139] a) Preparation of 1,2-dibromoacenaphthylene: under an argon atmosphere, in a Schlenk bottle, successively load 10 mmol of acenaphthene (Saen Chemical Technology (Shanghai) Co., Ltd.), 30 mmol of bromosuccinimide , 0.1 mmol of benzoyl peroxide, 25 mL of carbon tetrachloride was added to dissolve the reactants, and the reaction was carried out at 75° C. for 4 hours. After cooling, quench the reaction with aqueous sodium thiosulfate solution, extract the reaction solution with dichloromethane, dry the organic phase with anhydrous sodium sulfate, remove the organic phase solvent, and carry out column chromatography with petroleum ether as a developing solvent (Rf=0.9) to obtain 1,2-Dibromoacenaphthylene, the yield is 61%.
[0140] b) Preparation of 1-bromo-2-iodo-acenaphthylenene: Dissolve 5 mmol of 1,2-dibromoacenaphthylenene in 15 mL of anhydrous THF in a Schlenk bottle under a...
Embodiment 2
[0144] Preparation of (1-(2-methylphenyl)acenaphthenyl)-bis(3,5-bis(trifluoromethyl))phenylphosphine
[0145] a) Preparation of 1,2-dibromoacenaphthylene: under an argon atmosphere, in a Schlenk bottle, successively load 10 mmol of acenaphthene (Saen Chemical Technology (Shanghai) Co., Ltd.), 30 mmol of bromosuccinimide , 0.1 mmol of benzoyl peroxide, 25 mL of carbon tetrachloride was added to dissolve the reactant, and the reaction was refluxed at 75° C. for 4 hours. After cooling, the reaction was quenched with aqueous sodium thiosulfate solution, the reaction solution was extracted with dichloromethane, the organic phase was dried over anhydrous sodium sulfate, the organic phase solvent was removed, and column chromatography was carried out with petroleum ether as a developing solvent (Rf=0.9) to obtain 1 , 2-Dibromoacenaphthylene, the yield is 61%.
[0146] b) Preparation of 1-bromo-2-iodo-acenaphthylenene: Dissolve 5 mmol of 1,2-dibromoacenaphthylenene in 15 mL of anhydr...
Embodiment 3
[0150] Preparation of (1-(naphthyl)acenaphthenyl)-bis(3,5-bis(trifluoromethyl))phenylphosphine
[0151] a) Preparation of 1,2-dibromoacenaphthylene: under an argon atmosphere, in a Schlenk bottle, successively load 10 mmol of acenaphthene (Saen Chemical Technology (Shanghai) Co., Ltd.), 30 mmol of bromosuccinimide , 0.1 mmol of benzoyl peroxide, 25 mL of carbon tetrachloride was added to dissolve the reactants, and the reaction was carried out at 75° C. for 4 hours. After cooling, quench the reaction with aqueous sodium thiosulfate solution, extract the reaction solution with dichloromethane, dry the organic phase with anhydrous sodium sulfate, remove the organic phase solvent, and carry out column chromatography with petroleum ether as a developing solvent (Rf=0.9) to obtain 1,2-Dibromoacenaphthylene, the yield is 61%.
[0152] b) Preparation of 1-bromo-2-iodo-acenaphthylenene: Dissolve 5 mmol of 1,2-dibromoacenaphthylenene in 15 mL of anhydrous THF in a Schlenk bottle under...
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