4-(2,4-二氯苯氧基)-1-(二甲氨基)戊-1-烯-3-one

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A solution of 4-(2,4-dichlorophenoxy)-1-(dimethylamino)-1-penten-3-one (2.9 g) in glacial acetic acid (25 ml) was added to a stirred solution of 3-amino-1,2,4-triazole (0.93 g) also in glacial acetic acid (25 ml). The mixture was heated under reflux for 5 hours and then cooled to room temperature. The mixture was then poured into 200 ml of ice-water and extracted with toluene. The toluene extracts were washed with a 10% aqueous solution of sodium hydrogen carbonate followed by water, then dried over anhydrous magnesium sulphate and the solvent was evaporated under reduced pressure. The residue was triturated with cold diethyl ether and the solid was collected by filtration, followed by recrystallisation from a mixture of ethyl acetate and petroleum ether (b.p. 40°-60° C.) to give 7-[1-(2,4-dichlorophenoxy)ethyl]-1,2,4-triazolo[1,5-a]pyrimidine. Yield 2.02 g, (mp 137°-138° C.). The mixture was heated under reflux for 5 hours extracted with toluene The toluene extracts were washed with a 10% aqueous solution of sodium hydrogen carbonate dried over anhydrous magnesium sulphate the solvent was evaporated under reduced pressure The residue was triturated with cold diethyl ether the solid was collected by filtration followed by recrystallisation from a mixture of ethyl acetate and petroleum ether (b.p. 40°-60° C.)

反应条件: temp:120.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: A mixture of 3-(2,4-dichlorophenoxy)-2-butanone (4.66 g) and N,N-dimethylformamide dimethylacetal (2.38 g) was heated under argon in an oil bath at 120° C. for 11 hours. The methanol produced in the reaction was removed under reduced pressure and the residue was triturated with n-hexane. The solid was collected by filtration and washed with cold diethyl ether to give 4-(2,4-dichlorophenoxy)-1-(dimethylamino)-1-penten-3-one. Yield 4.07 g. was removed under reduced pressure the residue was triturated with n-hexane The solid was collected by filtration washed with cold diethyl ether