Synthesis method of bupirimate
A pyrithrimolsulfonate and synthetic method technology, applied in the direction of organic chemistry, can solve the problems of easy decomposition, floating reaction yield, large products, etc., and achieve the effect of stable yield and complete reaction of raw materials
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Embodiment 1
[0030] First, 100 g of pyrimol was dissolved in 200 ml of methanol, 19 g of sodium hydroxide was added, and the reaction was stirred at 25° C. for 1 hour. After stirring, methanol was evaporated to dryness. Afterwards, 300 mL of toluene and 82 g of N,N-dimethylsulfamoyl chloride were sequentially added to the reaction system, and the system was heated to reflux. After reacting for 8 hours, the toluene was evaporated to dryness, 300 mL of petroleum ether was added, the system was cooled to 0° C., and the product was stirred to precipitate; the product was centrifugally filtered, dried and weighed 143 g, and the yield was 95%.
[0031] 1 H NMR (500MHz, CDCl 3 )δ4.96(brs,0.9H),3.58-3.30(m,2H),3.05(s,6H),2.62-2.42(m,2H),2.34(s,3H),1.55-1.42(m,2H ),1.41-1.33(m,2H),1.21(t,J=7.2Hz,3H),0.94(t,J=7.2Hz,3H). 13 C NMR (126MHz, CDCl 3 )δ169.16, 163.16, 159.75, 110.43, 38.77, 36.40, 31.65, 24.73, 22.63, 21.83, 14.85, 13.90.
[0032] According to the above characterization data, it can...
Embodiment 2
[0034] First, 100 g of pyrimol was dissolved in 200 ml of ethanol, 51 g of sodium carbonate was added, and the reaction was stirred at 25° C. for 1 hour. After stirring, ethanol was evaporated to dryness. Afterwards, 300 mL of toluene and 82 g of N,N-dimethylsulfamoyl chloride were sequentially added to the reaction system, and the system was heated to reflux. After reacting for 8 hours, evaporate toluene to dryness, add petroleum ether 300mL, cool the system to 0°C, stir and precipitate the product; the product is filtered, dried and weighed 147g, which is pyrimetholsulfonate with a yield of 97%.
Embodiment 3
[0036] First, 100 g of pyrimol was dissolved in 200 ml of ethanol, 26 g of sodium methoxide was added, and the reaction was stirred at 25° C. for 1 hour. After stirring, ethanol was evaporated to dryness. Afterwards, 300 mL of toluene and 82 g of N,N-dimethylsulfamoyl chloride were sequentially added to the reaction system, and the system was heated to reflux. After reacting for 8 hours, evaporate the toluene to dryness, add petroleum ether 300mL, cool the system to 0°C, stir and precipitate the product; the product is centrifugally filtered, dried and weighed 140g, which is pyrimolsulfonate with a yield of 93%.
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