Aluminum compound with double five-membered chelating ring structure, its synthesis method and use
A technology of aluminum compounds and synthesis methods, applied in the fields of compounds containing group 3/13 elements of the periodic table, chemical instruments and methods, organic chemistry, etc., can solve the problems of further improvement of catalytic activity
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Embodiment 1
[0061] Synthesis of 1,2-bis(cycloheptatrienol)-phthalimine (SP-NH)
[0062]
[0063] Under nitrogen, add tris(dibenzylidene-BASE acetone)dipalladium (45.8 mg, 0.05 mmol, purchased from Anaiji Company), 1,1'-binaphthyl-2, 2'-bisdiphenylphosphine (62.3 mg, 0.1 mmol, purchased from Anaiji Company), cesium carbonate (4.56 g, 14 mmol, purchased from Anaiji Company), 2-trifluoromethanesulfonate ring Heptatrienone (6.1 g, 24 mmol), o-phenylenediamine (1.08 g, 10 mmol, purchased from Anaiji Company) and 50 ml of toluene.
[0064] The resulting mixture was stirred at 100°C for 24 hours, cooled to room temperature after the reaction was completed, and the toluene-insoluble solid was filtered out with diatomaceous earth, and 100 mesh silica gel was added to the obtained solution, which was spin-dried and sampled, and then the obtained crude product was passed through 200 - 300-mesh silica gel column, using petroleum ether: ethyl acetate = 3:1 (volume ratio) as eluent, spin-dried elue...
Embodiment 2
[0068] Synthesis of 1,2-bis(cycloheptatrienol)-phthalimine aluminum compound (SP-AlCl)
[0069]
[0070] Under nitrogen, the ligand prepared in Example 1 (1.58 g, 5 mmol) and 25 ml of toluene were added to a Schlenk bottle with a magnet. After dissolving, at room temperature, 0.9 moles per liter of diethylaluminum chloride toluene solution (4.5 milliliters, 5 mmol) was slowly injected into the reaction system with a syringe under nitrogen protection. After the addition, the reaction system was stirred at room temperature for 2 After that, it was placed in an oil bath, heated to 100°C and stirred for 12 hours, and a yellow solid was observed to precipitate.
[0071] After the reaction was completed and down to room temperature, the Schlenk bottle was brought into the glove box, the resulting mixture was filtered, the insoluble solid was washed three times with n-hexane, after which the solid was sucked dry, and the brownish yellow product (1.78 g, 95% yield) was collected. ...
Embodiment 3
[0076] Synthesis of 1,1'-bis(tropolone)binaphthyldiimide (SN-NH)
[0077]
[0078] Under nitrogen, add tris(dibenzylidene-BASE acetone)dipalladium (37 mg, 0.04 mmol, purchased from Anaiji Company), 1,1'-binaphthyl-2, 2'-bisdiphenylphosphine (50 mg, 0.08 mmol, purchased from Anaiji Company), cesium carbonate (3.65 g, 11.2 mmoles, purchased from Anaiji Company), 2-trifluoromethanesulfonate ring Heptatrienone (4.88 g, 19.2 mmol), 1,1'-bi-2-naphthylamine (2.27 g, 8 mmol, purchased from Anaiji Company) and 50 ml of toluene.
[0079] The resulting mixture was stirred at 100°C for 24 hours, cooled to room temperature after the reaction was completed, and the toluene-insoluble solid was filtered out with diatomaceous earth, and 100 mesh silica gel was added to the obtained solution, which was spin-dried and sampled, and then the obtained crude product was passed through 200 - 300 mesh silica gel column, using ethyl acetate as eluent, spin-dried eluent to obtain a brown solid (2.68...
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