Pyridyl phenylurea preparation method
A technology of pyridylphenylurea and pyridine, which is applied in the field of crop growth regulators, can solve the problems of high market price, high cost of large-scale production, cumbersome operation of high-purity CPPU products, etc., and achieve high yield and product purity, reduce Cost of production, availability of non-toxic or toxic effects
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Embodiment 1
[0023] The preparation method of present embodiment 1 is as follows:
[0024] 1. Add 120g of pyridine, 500ml of glacial acetic acid and 200ml of 36% hydrogen peroxide into a 3500ml three-necked flask, heat at 80 for 3 hours, then add 200ml of hydrogen peroxide, continue heating for 6 hours, concentrate under reduced pressure to 500ml, add Add 300ml of water, and add solid sodium carbonate to saturation, cool at room temperature and filter off the insoluble matter, and dry the filtrate with sodium sulfate to obtain 130g of the product, with a boiling point of 139-141°C.
[0025] 2. Dissolve 100g of pyridine oxide in a mixture of 120g of concentrated nitric acid and 300ml of concentrated sulfuric acid, heat in an oil bath at 128-130°C for 5 hours, pour it into crushed ice after natural cooling, add small amounts of solid sodium carbonate several times, and precipitate The crystals were washed with ice water and filtered to obtain 120 g of 4-nitropyridine nitrogen oxide with a me...
Embodiment 2
[0029] Add 700g of 4-nitropyridine nitrogen oxide (5mol) into a 5000ml three-necked flask, then add 400g of POCl 3 (2.6mol), heated to reflux for 3.5 hours, cooled to precipitate 2-chloro-4-nitropyridine, and dried to obtain 658g of the product, with a yield of 83.5%.
Embodiment 3
[0031] Add 40g of 4-nitropyridine nitrogen oxide (1mol) into a 500ml three-necked flask and then add 250g of SOCl 2 , heated up to 70° C., stirred, kept warm for 2.5 hours, cooled, 2-chloro-4-nitropyridine was precipitated, and dried to obtain 126 g of the product with a yield of 80%.
[0032] Other steps of above-mentioned embodiment 2, embodiment 3 are the same as embodiment 1.
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