Method for producing verelite with [O,N] type catalyst of bidentate ligand coordinated with post-transition metal
A late-transition metal and bidentate ligand technology, applied in the chemical industry, can solve the problems of lack of stereoregularity and limit the use of polystyrene, and achieve good catalytic activity
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Embodiment 1
[0021] Example 1 Preparation of Ligand 7-hydroxyindan-1-(N-phenylimine)
[0022] in N 2 Next, 1.68g (11.4mmol) of 7-hydroxyindanone and 1.4mL (15.0mmol) of aniline were added to a 100mL three-necked flask, and then 30mL of absolute ethanol, 0.1mL of formic acid, and 0.7g of 4A molecular sieves were added. Heat to reflux for 48 hours. After the end of the reaction, filter, collect the filtrate, and use anhydrous Mg 2 SO 4 It was dried, concentrated, and passed through a silica gel column using a mixed solution of petroleum ether and ethyl acetate as an eluent to obtain 1.53 g of an orange oil with a yield of 60%.
Embodiment 2
[0023] Example 2 Preparation of Ligand 7-hydroxy-3,4-dimethyl-6-tert-butylindan-1-(N-phenylimine)
[0024] in N 2 1.3mL (11.4mmol) TiCl will be dissolved within 30min 4 30mL of toluene solution was added to 40mL of toluene solution containing 4.3mL (45.4mmol) aniline. Then the reaction mixture was heated to 90° C., and 2.63 g (11.4 mmol) of 7-hydroxy-3,4-dimethyl-6-tert-butylindanone was added after 30 min. At this temperature, the reaction was carried out for 48 hours. After the reaction, the reaction solution was poured into Na 2 CO 3 Saturated aqueous solution, liquid separation, organic phase with anhydrous Mg 2 SO 4 It was dried, concentrated, and passed through a silica gel column using a mixed solution of petroleum ether and ethyl acetate as an eluent to obtain 2.75 g of an orange-red solid with a yield of 45%.
Embodiment 3
[0025] The preparation of the catalyst of embodiment 3 and metal Ni coordination
[0026] 0.122g (0.49mmol) of Ni(OAc) 2 4H 2 O and 0.327g (0.98mmol) of 7-hydroxy-3,4-dimethylindan-1-(N-2,6-diisopropylphenylimine) were added to 20mL of absolute ethanol, and heated to reflux for 3 hours. After cooling, the solid was collected by filtration and dried under vacuum. 0.236 g of a tan solid was obtained with a yield of 75%.
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