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With Ni(1,5-cyclooctadiene)2; In tetrahydrofuran; diethyl ether; at 110℃; for 4.5h;Microwave irradiation;
The 3-chloro-4-aminopyridine was mixed with tetrahydrofuran and added to the reactor. The mixture was heated to 110 C., and diethyl ether and Ni(COD) 2 were added. The catalyst was added. Under stirring, acetylene was added to perform microwave irradiation for 30 minutes.Afterwards, refluxing reaction was continued for 4 hours. After the reaction was completed, filtration was performed. The filtrate was evaporated off to tetrahydrofuran, extracted with ethyl acetate, recrystallized with water, suction filtered and dried to obtain 5-azaindole;The catalyst is a molybdenum trioxide-alumina composite. The catalyst is prepared by dissolving ammonium molybdate in water, adding alumina particles, ultrasonically dispersing, adding urea, and adding hydrochloric acid dropwise under stirring conditions.After completion of the dropwise addition, the precipitate was filtered, washed, dried and calcined at 400 C. to obtain a molybdenum trioxide-alumina composite.The molar ratio of ammonium molybdate and urea is 1:0.5;The molar ratio of hydrochloric acid to ammonium molybdate is 1:1;The molar ratio of molybdenum trioxide to alumina in the molybdenum trioxide-alumina composite is 1:3. The 3-chloro-4-aminopyridine and ether molar ratio of 2:1.5;The molar ratio of 3-chloro-4-aminopyridine to Ni(COD)2 is 7:2;The molar ratio of 3-chloro-4-aminopyridine to acetylene is 1:1.5;The mass ratio of 3-chloro-4-aminopyridine to the catalyst is 12:11;The microwave radiation power is 300W.The yield of the obtained 5-azaindole was 90.4% and the purity was 99.1%.
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