A kind of anti-inflammation compound and preparation method thereof
A compound, C1-C6 technology, applied in anti-inflammatory agents, organic chemistry, drug combination, etc.
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Embodiment 1
[0082] The reaction route is:
[0083]
[0084] Specifically include the following steps:
[0085] S1: Add 100 mmol of the compound of the above formula (1), 50 mmol of the compound of the above formula (2) and 300 mmol of potassium carbonate to an appropriate amount of organic solvent dimethyl sulfoxide (DMSO) in the reaction vessel, and stir and react at 80°C for 16 hours;
[0086] After the reaction, the reaction mixture was poured into water and extracted twice with ethyl acetate, the organic phases were combined, washed with water and washed with anhydrous Na 2 SO 4 Drying, distillation under reduced pressure, the resulting residue was eluted by silica gel flash column chromatography (a mixture of dichloromethane and ethyl acetate with a volume ratio of 50:1 as eluent), and the eluate was collected and evaporated to remove the eluent. reagent, thereby obtaining the compound of the above formula (3) as a white solid with a yield of 96.1%.
[0087] 1 H NMR (500MHz, D...
Embodiment 2
[0097] Reaction scheme is with embodiment 1.
[0098] Specifically include the following steps:
[0099] S1: Add 100 mmol of the compound of formula (1), 150 mmol of the compound of formula (2) and 200 mmol of potassium carbonate to an appropriate amount of organic solvent dimethyl sulfoxide (DMSO) in the reaction vessel, and stir the reaction at 120°C for 8 Hour;
[0100] After the reaction, the reaction mixture was poured into water and extracted twice with ethyl acetate, the organic phases were combined, washed with water and washed with anhydrous Na 2 SO 4 Drying, distillation under reduced pressure, the resulting residue was eluted by silica gel flash column chromatography (a mixture of dichloromethane and ethyl acetate with a volume ratio of 50:1 as eluent), and the eluate was collected and evaporated to remove the eluent. reagent, thereby obtaining the compound of formula (3) as a white solid with a yield of 95.8%.
[0101] The NMR characterization data are the same...
Embodiment 3
[0109] Reaction scheme is with embodiment 1.
[0110] Specifically include the following steps:
[0111] S1: Add 100 mmol of the compound of formula (1), 100 mmol of the compound of formula (2) and 250 mmol of potassium carbonate to an appropriate amount of organic solvent dimethyl sulfoxide (DMSO) in the reaction vessel, and stir the reaction at 100°C for 12 Hour;
[0112] After the reaction, the reaction mixture was poured into water and extracted twice with ethyl acetate, the organic phases were combined, washed with water and washed with anhydrous Na 2 SO 4 Drying, distillation under reduced pressure, the resulting residue was eluted by silica gel flash column chromatography (a mixture of dichloromethane and ethyl acetate with a volume ratio of 50:1 as eluent), and the eluate was collected and evaporated to remove the eluent. reagent, thereby obtaining the compound of formula (3) as a white solid with a yield of 96.4%.
[0113] The NMR characterization data are the sam...
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