Asymmetric preparation method of pyridinol nitrogen oxide
A nitrogen oxide and pyridyl alcohol technology, applied in the field of preparation of pyridyl alcohol nitrogen oxides, can solve the problems of inability to meet industrial production, large influence of ee value, single catalytic system, etc., and achieves great implementation value and social and economic benefits, Simple operation and high atom economy effect
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Embodiment 1
[0038] Embodiment 1 (ligand investigation)
[0039]
[0040] In an argon-protected glove box, weigh 0.021 mmol of the chiral ligand L* and the metal M precursor [Ir(COD)Cl] 2 (0.01mmol, 6.7mg) was added to a 10mL volumetric flask, 2mL of isopropanol solution was added, and stirred at room temperature for 1 hour until it was completely dissolved. The catalyst solution could be directly used for homogeneous catalytic hydrogenation reaction.
[0041] Under argon atmosphere, sequentially add compound 1a (0.2mmol, 40mg), potassium carbonate (0.002mmol, 0.3mg) and prepared catalyst solution (20μL, 0.0002mmol) into a 5mL hydrogenation tube, and then add 1mL of isopropyl Alcohol, put the reaction tube in an autoclave, replace the gas in the autoclave with hydrogen three times, and finally fill with 50atm hydrogen, and react in a constant temperature oil bath at 50°C for 12 hours. After the reaction, the gas in the autoclave was slowly released, the reaction mixture was purified wi...
Embodiment 2
[0045] Embodiment 2 (solvent investigation)
[0046]
[0047]
[0048] In an argon-protected glove box, weigh 0.021 mmol of chiral ligand III-3 and metal M precursor [Ir(COD)Cl] 2 (0.01mmol, 6.7mg) was added to a 10mL volumetric flask, 2mL of isopropanol solution was added, and stirred at room temperature for 1 hour until it was completely dissolved. The catalyst solution could be directly used for homogeneous catalytic hydrogenation reaction.
[0049] Under argon atmosphere, sequentially add compound 1a (0.2mmol, 40mg), potassium carbonate (0.002mmol, 0.3mg) and prepared catalyst solution (20μL, 0.0002mmol) into a 5mL hydrogenation tube, and then add 1mL of solvent, The reaction tube was placed in an autoclave, and the gas in the autoclave was replaced with hydrogen for three times, and finally filled with 50 atm of hydrogen, and reacted in a constant temperature oil bath at 25°C for 0.5 hours. After the reaction, the gas in the autoclave was slowly released, the react...
Embodiment 3
[0052] Embodiment 3 (the investigation of alkali)
[0053]
[0054]
[0055] In an argon-protected glove box, weigh 0.021 mmol of chiral ligand III-3 and metal M precursor [Ir(COD)Cl] 2 (0.01mmol, 6.7mg) was added to a 10mL volumetric flask, 2mL of isopropanol solution was added, and stirred at room temperature for 1 hour until it was completely dissolved. The catalyst solution could be directly used for homogeneous catalytic hydrogenation reaction.
[0056] Under argon atmosphere, sequentially add compound 1a (0.2mmol, 40mg), base (0.002mol) and prepared catalyst solution (20μL, 0.0002mmol) into a 5mL hydrogenation tube, then add 1mL isopropanol, and react The tube was placed in an autoclave, and the gas in the autoclave was replaced with hydrogen three times, and finally filled with 50 atm hydrogen, and reacted in a constant temperature oil bath at 25°C for 12 hours. After the reaction, the gas in the autoclave was slowly released, the reaction mixture was purified wi...
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