A kind of synthetic method of aromatic ring pyridine compound
A synthetic method and compound technology, applied in the direction of organic chemistry, etc., can solve the problems of difficult availability of raw materials, poor atom economy, high environmental factors, etc., and achieve the effects of wide application range, simple operation, and avoiding environmental pollution
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Embodiment 1
[0031]
[0032] Add 1a (0.5mmol, 60.5mg), chlorobenzene (3mL), Cu(OAc) into a 15mL reaction tube 2 (0.05 mmol, 9.1 mg), 2,2'-bipyridine (0.1 mmol, 15.6 mg), TEMPO (0.5 mmol, 78.1 mg) and 2a (0.6 mmol, 80.0 μL). After evacuating and filling with nitrogen, the reaction tube was sealed, and placed in an oil bath at 120° C. for a stirring reaction for 16 h. Stop the reaction, add 15mL of dichloromethane, then wash with water and saturated NaCl solution successively, and wash the organic phase with anhydrous MgSO 4 dry. Filtration, spin-drying, and silica gel column separation (petroleum ether / ethyl acetate=10 / 1) gave the target product 3a (46.6 mg, 40%). The characterization data of this compound are as follows: 1 H NMR (400MHz, CDCl 3 )δ7.50-7.54(m,2H),7.59-7.66(m,2H),7.81-7.83(m,1H),7.85(dd,J 1 =8.4Hz,J 2 =1.2Hz, 2H), 7.89(d, J=8.4Hz, 1H), 8.18(d, J=8.0Hz, 1H), 8.53(d, J=2.0Hz, 1H), 9.32(d, J=2.4 Hz,1H). 13 C NMR (100MHz, CDCl 3 )δ126.6, 127.6, 128.6, 129.2, 129.5, 1...
Embodiment 2
[0034] Add 1a (0.5mmol, 60.5mg), toluene (3mL), Cu(OAc) into a 15mL reaction tube 2 (0.05 mmol, 9.1 mg), 2,2'-bipyridine (0.1 mmol, 15.6 mg), TEMPO (0.5 mmol, 78.1 mg) and 2a (0.6 mmol, 80.0 μL). After evacuating and filling with nitrogen, the reaction tube was sealed, and placed in an oil bath at 120° C. for a stirring reaction for 16 h. Stop the reaction, add 15mL of dichloromethane, then wash with water and saturated NaCl solution successively, and wash the organic phase with anhydrous MgSO 4 dry. Filtered, spin-dried, separated by silica gel column (petroleum ether / ethyl acetate=10 / 1) to obtain the target product 3a (48.9 mg, 42%).
Embodiment 3
[0036] Add 1a (0.5mmol, 60.5mg), 1,4-dioxane (3mL), Cu(OAc) into a 15mL reaction tube 2 (0.05 mmol, 9.1 mg), 2,2'-bipyridine (0.1 mmol, 15.6 mg), TEMPO (0.5 mmol, 78.1 mg) and 2a (0.6 mmol, 80.0 μL). After evacuating and filling with nitrogen, the reaction tube was sealed, and placed in an oil bath at 120° C. for a stirring reaction for 16 h. Stop the reaction, add 15mL of dichloromethane, then wash with water and saturated NaCl solution successively, and wash the organic phase with anhydrous MgSO 4 dry. Filtration, spin-drying, and silica gel column separation (petroleum ether / ethyl acetate=10 / 1) gave the target product 3a (44.3 mg, 38%).
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