Compound taking triarylamine as core, and preparation method and application of compound
A compound, triarylamine technology, applied in chemical instruments and methods, condensation/addition reaction to prepare amino compounds, organic chemistry, etc., can solve very different problems
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Embodiment 1
[0085] Embodiment 1: the synthesis of reactant I
[0086]
[0087] Step 1: take raw material I and intermediate I as raw material, ethanol and toluene as solvent, wherein, the ratio of described toluene and ethanol is 2:(0.8-1.2), and the amount of toluene is that every gram of raw material I uses 30-50ml, so The molar ratio of raw material I and intermediate I is 1:(1.0-1.5); Pd(PPh 3 ) 4 And potassium carbonate, make reaction system; Wherein, described Pd(PPh 3 ) 4 The molar ratio to the raw material I is (0.005~0.01):1, and the potassium carbonate and water are configured to obtain a 2-2.5mol / L aqueous solution; under the protection of nitrogen, the reaction system is reacted at 95~110°C for 10~24 hours , naturally cooled to room temperature, and filtered the reaction solution, and the filtrate was subjected to vacuum rotary evaporation, and passed through a neutral silica gel column to obtain intermediate II;
[0088] Step 2: Dissolve intermediate II with 50-80mL of...
Embodiment 2
[0095] Embodiment 2: the synthesis of intermediate I
[0096]
[0097] Under nitrogen atmosphere, weigh raw material III, bis(pinacolate) diboron, Pd(dppf)Cl 2 1. Potassium acetate was dissolved in toluene, reacted at 100-120°C for 12-24 hours, sampled and plated, the reaction was complete, cooled naturally, filtered, and the filtrate was rotary evaporated to obtain a crude product, which was passed through a neutral silica gel column to obtain intermediate I; raw material The molar ratio of Ⅲ to bis(pinacolate) diboron is 2:(1~1.5), the raw material Ⅲ and Pd(dppf)Cl 2 The mol ratio of the raw material III is 1:(0.01~0.05), and the mol ratio of raw material III and potassium acetate is 1:(2~2.5);
[0098] Take intermediate I-1 as an example:
[0099]
[0100] Under a nitrogen atmosphere, weigh 0.02mol of raw material III-1, 0.012mol of bis(pinacolate) diboron, 0.0002mol of Pd(dppf)Cl 2 1. Dissolve 0.05mol potassium acetate in toluene, react at 100-120°C for 12-24 hour...
Embodiment 3
[0101] Embodiment 3: the synthesis of reactant III
[0102]
[0103] Weigh the intermediate reactant II and raw material IV, dissolve with toluene; then add Pd 2 (dba) 3 , P(Ph) 3 , sodium tert-butoxide; under an inert atmosphere, react the mixed solution of the above-mentioned reactants at 95-110° C. for 10-24 hours, cool and filter the reaction solution, spin the filtrate, and pass through a silica gel column to obtain intermediate IV; The molar ratio of reactant II and raw material IV is 1:(1.0~1.5), Pd 2 (dba) 3 The molar ratio with reactant II is (0.006~0.02):1, P(Ph) 3 The molar ratio to reactant II is (0.006~0.02):1, and the molar ratio of sodium tert-butoxide to reactant II is (1.0~3.0):1;
[0104] Under nitrogen atmosphere, weigh intermediate IV, bis(pinacolate) diboron, Pd(dppf)Cl 2 1. Potassium acetate was dissolved in toluene, reacted at 100-120°C for 12-24 hours, sampled and spotted on a plate, the reaction was complete, cooled naturally, filtered, and th...
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