A method for preparing 2-[phenyl]-1,2,4-triazine-3,5(2h,4h)-dione compounds
A technology of compounds and diketones, which is applied in the field of veterinary medicine, can solve the problems of high unit consumption of raw materials, low product purity, and low yield, and achieve the effects of shortening the reaction steps, improving economic benefits, and reducing emissions
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Embodiment 1
[0029] (1) Add 720g of toluene to a 1000ml four-necked bottle, add 120g of dichloroacetyl chloride, 25.89g of 0.3 equivalent of sodium carbonate, and accurately drop 79.79g of 1.1 equivalent of molten ethyl carbamate using a peristaltic pump for 0.5h. Insulate at 65°C, monitor the end of the reaction by liquid phase monitoring, and isolate (2,2-dichloroacetyl) ethyl carbamate 156.27g after the end of the reaction, with a yield of 93.20% and a purity of 97.13%;
[0030] (2) Add 500g of N-(4-(4-amino-2-methylphenoxy)phenyl)acetamide into a 10000ml four-necked flask, add 2250g of hydrochloric acid, cool down to 5-15°C, and add 1.05 equivalents dropwise 20wt% sodium nitrite aqueous solution 706.61g, after 0.5 hours of dropping, keep warm for 1h and the reaction is completed, add 3.5 equivalents of 20wt% sodium bisulfite aqueous solution 3552.44g to a 10000ml four-neck flask and heat up to 90°C, and the above diazotized feed solution Use a peristaltic pump to add dropwise to the aq...
Embodiment 2
[0033] (1) Add 720g of p-xylene to a 1000ml four-necked bottle, add 120g of dichloroacetyl chloride, 47.46g of 0.55 equivalent of sodium carbonate, and accurately drop 79.79g of 1.1 equivalent of molten ethyl carbamate using a peristaltic pump, dropwise adding 0.5 h, keep warm at 65°C, monitor the end of the reaction by liquid phase monitoring, and isolate (2,2-dichloroacetyl) ethyl carbamate 159.41g after the end of the reaction, with a purity of 96.25% and a yield of 94.21%;
[0034] (2) Add 500g of N-(4-(4-amino-2-methylphenoxy)phenyl)acetamide into a 10000ml four-necked flask, add 2250g of hydrochloric acid, cool down to 5-15°C, and add 1.05 equivalents dropwise 20wt% sodium nitrite aqueous solution 706.61g for 0.5 hours, after the dropwise addition, keep warm for 1h and the reaction is completed. Add 3.5 equivalents of 20wt% sodium bisulfite aqueous solution 3552.44g to a 10000ml four-neck flask and heat up to 90°C. The solution was added dropwise to the aqueous solution ...
Embodiment 3
[0037] (1) Add 720g of m-xylene to a 1000ml four-necked bottle, add 120g of dichloroacetyl chloride, 47.46g of 0.55 equivalent of sodium carbonate, and accurately drop 79.79g of 1.1 equivalent of molten ethyl carbamate using a peristaltic pump, drop 0.5 h, keep warm at 65°C, monitor the end of the reaction by liquid phase monitoring, and isolate (2,2-dichloroacetyl) ethyl carbamate 156.84g after the end of the reaction, with a purity of 95.71% and a yield of 92.17%;
[0038] (2) Add 500g of N-(4-(4-amino-2-methylphenoxy)phenyl)acetamide into a 10000ml four-necked flask, add 2250g of hydrochloric acid, cool down to 5-15°C, and add 1.05 equivalents dropwise 20wt% sodium nitrite aqueous solution 706.61g for 0.5 hours, after the dropwise addition, keep warm for 1h and the reaction is completed. Add 3.5 equivalents of 20wt% sodium bisulfite aqueous solution 3552.44g to a 10000ml four-neck flask and heat up to 90°C. The solution was added dropwise to the aqueous solution of sodium b...
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