A kind of method for preparing aza seven-membered ring benzazepine compounds by visible light catalysis
A technology for the preparation of benzazepine and catalysis, which is applied in the field of catalytic synthesis, can solve problems such as unfavorable reaction universality, operation, large-scale application of limiting schemes, harsh reaction conditions, etc., and achieve good yield, wide application range, and reaction The effect of system saving
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Embodiment 1
[0036] Dissolve 0.25 mmol of pyridine-N-oxide and 0.25 mmol of trifluoroacetic anhydride in 6 mL of dichloromethane to obtain a dichloromethane solution; use Ru(bpy) 3 Cl 2 ·6H 2 O( Tris(2,2'-bipyridyl)ruthenium chloride hexahydrate ) is a visible light catalyst, and 0.8 mg of this catalyst is added to a dichloromethane solution; 0.1 mmol of alkynylamine compound-1(R 1 , R 2 , R 3 , R 4 , R 5 , R 6 , R 7 , R 8 , R 9 for H, R 10 for CF 3 CO) was added to the dichloromethane solution. The concentration of photosensitizer is 1.7×10 -4 M. Argon was used to deoxygenate for 10 min, and then irradiated with 450 nm±10 nm Blue LEDs for 9 h at room temperature under the stirring of a magnetic stirrer. After the reaction, the solvent was removed by distillation under reduced pressure, and the corresponding product was obtained by thin-layer chromatography. It was identified as aza-seven-membered ring benzazepine product-2(R 1 , R 2 , R 3 , R 4 , R 5 , R 6 , R 7 , R...
Embodiment 2
[0038] Same as Example 1, the difference is: add 1.5mg visible light catalyst, the concentration of photosensitizer is 3.3×10 -4 M. The product is aza seven-membered ring benzazepine products-2(R 1 , R 2 , R 3 , R 4 , R 5 , R 6 , R 7 , R 8 , R 9 for H, R 10 for CF 3 CO, R 11 for CF 3 ). The yield of product was 73%.
Embodiment 3
[0040] Same as Example 1, the difference is: add 2.3mg visible light catalyst, the concentration of photosensitizer is 5.0×10 -4 M. The product is aza seven-membered ring benzazepine products-2(R 1 , R 2 , R 3 , R 4 , R 5 , R 6 , R 7 , R 8 , R 9 for H, R 10 for CF 3 CO, R 11 for CF 3 ). The yield of the product was 85%.
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