A kind of synthetic method of medicine intermediate quinazoline derivative
A synthesis method and quinazoline technology are applied in the field of synthesis of organic nitrogen-containing heterocyclic compounds, can solve the problems of difficult synthesis of o-aminobenzylamine, rare raw materials, use of precious metal catalysts, etc., and achieve good research value and industrial application prospects. Effect
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Embodiment 1
[0052]
[0053] Under an oxygen atmosphere, add 100mmol of the above formula (II) compound, 150mmol of the above formula (III) compound, 200mmol of ammonium chloride, 10mmol of CuI, 10mmol of 2,2'-bipyridyl, 10mmol of TEMPO, 5mmol of nitric acid to an appropriate amount of organic solvent acetonitrile Cerium ammonium and 200mmol KOH, the resulting system was stirred and reacted at 30°C for 12 hours, and then the temperature was raised and stirred at 80°C for 24 hours;
[0054] After the reaction was completed, the reaction system was cooled to room temperature, diluted with ethyl acetate, washed fully with saturated brine, then extracted with ethyl acetate for 2-3 times, the organic phases were combined, dried with anhydrous sodium sulfate, and then reduced Concentrate under reduced pressure, 300-400 mesh silica gel column chromatography on the residue, make eluent with the equal volume mixture of normal hexane and ethyl acetate, after eluent is concentrated, thus obtain the...
Embodiment 2
[0057]
[0058] Under an oxygen atmosphere, add 100mmol of the compound of the above formula (II), 200mmol of the compound of the above formula (III), 250mmol of ammonium chloride, 20mmol of CuI, 20mmol of 4,4'-bipyridine, 20mmol of TEMPO, and 10mmol of nitric acid to an appropriate amount of organic solvent acetonitrile Cerium ammonium and 250mmol KOH, the resulting system was stirred and reacted at 30°C for 12 hours, and then the temperature was raised and stirred at 80°C for 24 hours;
[0059] After the reaction was completed, the reaction system was cooled to room temperature, diluted with ethyl acetate, washed fully with saturated brine, then extracted with ethyl acetate for 2-3 times, the organic phases were combined, dried with anhydrous sodium sulfate, and then reduced Concentrate under reduced pressure, 300-400 mesh silica gel column chromatography on the residue, make eluent with the equal volume mixture of normal hexane and ethyl acetate, after eluent is concentra...
Embodiment 3
[0062]
[0063] Under an oxygen atmosphere, add 100mmol of the above formula (II) compound, 250mmol of the above formula (III) compound, 300mmol of ammonium chloride, 30mmol of CuI, 30mmol of 2,2'-bipyridyl, 30mmol of TEMPO, 15mmol of nitric acid to an appropriate amount of organic solvent acetonitrile Cerium ammonium and 300mmol KOH, the resulting system was stirred and reacted at 30°C for 12 hours, and then the temperature was raised and stirred at 80°C for 24 hours;
[0064] After the reaction was completed, the reaction system was cooled to room temperature, diluted with ethyl acetate, washed fully with saturated brine, then extracted with ethyl acetate for 2-3 times, the organic phases were combined, dried with anhydrous sodium sulfate, and then reduced Concentrate under reduced pressure, 300-400 mesh silica gel column chromatography on the residue, make eluent with the equal volume mixture of normal hexane and ethyl acetate, after eluent is concentrated, thus obtain th...
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