Prepn of pyrido-phenylurea
A technology of pyridylphenylurea and phenylurea, which is applied in the preparation of pyridylphenylurea N--N`-phenylurea, the field of phenylurea-type cytokinin high-efficiency plant growth regulator, can solve the problem of high market price, 2 - Problems such as high toxicity of chloropyridine and limited sources of raw materials, to achieve the effect of reducing production costs, non-toxic or low toxicity, and high product purity
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Embodiment 1
[0026] The preparation method of present embodiment 1 is as follows:
[0027] 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.
[0028] 2. Pass 310g of chlorine into 678g of pyridine oxide, CCl 4 In a mixture with water, the halogenation reaction was carried out under ultraviolet light for 3 hours, the resulting reactant was extracted with water, the extract was adjusted to pH 11 with 20% NaOH, then distilled and cooled to obtain 856 g of 2,4-dichloropyridine nitrogen oxide , yield 82.2%.
[0029] 3. Dissolve 120g of 2,4-dichloropyrid...
Embodiment 2
[0032] In a 3-liter reactor, under the protection of nitrogen, the chlorination reaction is carried out under the following conditions: pyridine: N: Cl 2 =1:1:2, the temperature is controlled at 165-170, when 249g of pyridine oxide is added, and chlorine is passed for 3 hours, an acidic mixture is obtained, and the pH is adjusted to 8.5-10.0 with ammonia water, and the solvent CCl is recovered 4 , to obtain product 2,4-dichloropyridine 411g, yield 94%
Embodiment 3
[0034] Chlorine gas is directly introduced into 83g of pyridine oxide, and 121g of 2,4-dichloropyridine is obtained at 0-5 to the end point, and the yield is 83%. If the temperature rises to 70°C, the product yield is 8%. increased, the product yield decreased.
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