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Solvent-free solid-phase synthesis method and application of microwave digestion of five-membered heterocyclic azoles containing oxygen, sulfur and nitrogen
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The technology of a compound and a cyclizing agent, applied in the application field of the three series of compounds, can solve the problems such as few reports on the application of organic synthesis
Inactive Publication Date: 2019-04-02
SOUTH CENTRAL UNIVERSITY FOR NATIONALITIES
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Embodiment 1～8
[0062] 1. Embodiment 1~8 is the synthesis of oxygen-containing substituted five-membered heterocyclic azole compounds
Embodiment 1
[0063] The synthesis of embodiment 1,2-indolyl-5-phenyloxazole (Ⅱa1)
[0064]
[0065] Weigh 2.78g of N-(2-oxo-2-phenyl)ethyl-1H-indole-3-carboxamide and 1.7g of phosphoruspentoxide in the glove box and put them in an agate mortar in the glove box , mix evenly, grind finely, transfer to a 10mL reaction bottle in a microwave reactor, adjust the power of the microwave reactor to 560W, start the microwave reactor and heat up from room temperature to 230°C at a heating rate of 45°C / min, then react at a constant temperature for 30 Minutes, close the microwave reactor, stop the reaction, cool down to room temperature naturally, wash the mixture in the reaction flask with distilled water, dry, recrystallize from ethanol, and weigh 2.33g (IIa1) as a pale white solid, with a yield of 89.7%. mp:188~190℃.IRν(cm -1 ):3413,3154,2919,1625,1602,1443,1361,1249,1120,914,767,726; 1 H-NMR(400MHz,DMSO-d6):8.10–8.07(m,2H),7.98–7.95(m,2H),7.60–7.48(m,5H),7.25–7.17(m,2H); 13 C-NMR (125MHz, DM...
Embodiment 2
[0067] The synthesis of embodiment 2,2-indolyl-5 pyridyl oxazole (IIa2)
[0068]
[0069] Weigh 2.78g of N-(2-oxo-2-pyridyl)ethyl-1H-indole-3-carboxamide in the glove box, measure 1.5mL of phosphorus oxychloride, put into 10mL of microwave reactor to react In the bottle, adjust the power of the microwave reactor to 500W, start the microwave reactor and raise the temperature from room temperature to 230°C at a heating rate of 45°C / min, then react at a constant temperature for 20 minutes, turn off the microwave reactor, stop the reaction, cool naturally to room temperature, and put the reaction The mixture in the bottle was washed with distilled water, dried, recrystallized from ethanol, and weighed to obtain 2.42 g of (IIa2) as a yellow solid with a yield of 93.0%. mp:179~181℃.IRν(cm -1 ):3173,2919,1755,1628,1431,1331,1255,1120,1008,920,803,750,703,614; 1 H-NMR (400MHz, DMSO-d 6 ):9.27(s,1H),8.69(d,J=5.0Hz,1H),8.41(d,J=6.7Hz,1H),8.01(d,J=2.4Hz,1H),7.97(d,J =7.9Hz,1H),7.6...
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Abstract
The invention belongs to the technical field of organic synthesis, and particularly discloses a microwave-digestionsolvent-free solid-phase synthesis method and an application of oxygen-containing, sulfur-containing and nitrogen-containing substituted five-membered heterocycle azole compounds. The microwave-digestionsolvent-free solid-phase synthesis method is adopted to synthesize a target object, microwavedigestion has two characteristics of closed container reaction and microwave heating, a cyclizing agent is gasified through high temperature and high pressure, produced aerosol dissolves a sample, a homogeneous reaction is performed, the synergistic effect of microwave radiation and the cyclizing agent determines the advantages of short reaction time, non-volatility of reaction raw materials, recyclability and the like, the production cost is effectively reduced, energy is saved, and the environment is protected; besides, the operation is simple, and the yield is higher. The three series of oxygen-containing, sulfur-containing and nitrogen-containing substituted five-membered heterocycle azole compounds prepared with the method have excellent photophysical properties in the aspects of fluorescence, ultraviolet and the like and has good antibacterial and insecticidal bioactivity, thereby having great development and application value and prospect.
Description
technical field [0001] The invention relates to the technical field of organic synthesis, in particular to three series of oxygen-containing, sulfur-containing and nitrogen-containing substituted five-membered heterocyclic azole compounds and their microwave digestionsolvent-free solid-phase synthesis method, as well as the application of the three series of compounds. Background technique [0002] Oxygen-containing, sulfur-containing, and nitrogen-containing substituted azole compounds are an important class of five-membered heterocyclic compounds. Due to their easy formation of hydrogen bonds, coordination with metal ions, and π-π stacking, electrostatic and hydrophobic interactions, oxygen, Sulfur-containing and nitrogen-containing substituted azole compounds can undergo a variety of non-covalent interactions and exhibit some special properties. In the field of materials, azole compounds can be applied to new materials in many fields such as photoluminescent materials, n...
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