A kind of synthetic method of pharmaceutical intermediate diarylethene compound
A synthesis method and compound technology are used in the synthesis of pharmaceutical intermediate diarylethene compounds and the synthesis of unsaturated olefin compounds, which can solve the problems of complicated catalyst preparation and difficult large-scale application, and achieve a good application basis and research. Value, effect of good technical effect
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Embodiment 1
[0043]
[0044] The specific reaction operation is as follows: at room temperature, add 100 mmol of the compound of the above formula (II), 100 mmol of the compound of the above formula (III), 1 mmol of palladium acetate, 80 mmol of tetra-n-butyl ammonium bromide and 250mmol sodium carbonate, then stirred and warmed up to 80°C, and stirred and reacted at this temperature for 30 hours;
[0045] After the reaction was finished, the reaction mixture was poured into a sufficient amount of ethyl acetate, then washed with saturated brine, and the organic layer and the water layer were separated. After the water layer was fully extracted with ethyl acetate, the organic layers were combined (after washing with saturated brine). The organic layer and the organic layer obtained by ethyl acetate extraction), with anhydrous Na 2 SO 4 Drying, distillation under reduced pressure, the residue is eluted by flash column chromatography (with a mixture of petroleum ether and ethyl acetate at...
Embodiment 2
[0048]
[0049] The specific reaction operation is: at room temperature, add 100mmol of the compound of the above formula (II), 200mmol of the compound of the above formula (III), 0.4mmol of palladium acetate, 150mmol of tetra-normal Butylammonium bromide and 150mmol sodium carbonate, then stirred and warmed up to 120°C, and stirred and reacted at this temperature for 15 hours;
[0050] After the reaction was finished, the reaction mixture was poured into a sufficient amount of ethyl acetate, then washed with saturated brine, and the organic layer and the water layer were separated. After the water layer was fully extracted with ethyl acetate, the organic layers were combined (after washing with saturated brine). The organic layer and the organic layer obtained by ethyl acetate extraction), with anhydrous Na 2 SO 4 Drying, distillation under reduced pressure, the residue is eluted by flash column chromatography (with a mixture of petroleum ether and ethyl acetate at a volu...
Embodiment 3
[0053]
[0054] The specific reaction operation is: at room temperature, add 100mmol of the compound of the above formula (II), 150mmol of the compound of the above formula (III), 0.8mmol of palladium acetate, 100mmol of tetra-normal Butyl ammonium bromide and 225mmol sodium carbonate, then stirred and warmed up to 95°C, and stirred and reacted at this temperature for 25 hours;
[0055] After the reaction was finished, the reaction mixture was poured into a sufficient amount of ethyl acetate, then washed with saturated brine, and the organic layer and the water layer were separated. After the water layer was fully extracted with ethyl acetate, the organic layers were combined (after washing with saturated brine). The organic layer and the organic layer obtained by ethyl acetate extraction), with anhydrous Na 2 SO 4 Drying, distillation under reduced pressure, the residue is eluted by flash column chromatography (with a mixture of petroleum ether and ethyl acetate at a volu...
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