Refining method of gimeracil
A refining method and crude product technology, applied in organic chemistry and other directions, can solve the problems of difficult removal of impurities, large amount of solvent, and many impurities, and achieve the effect of pure white product color, good impurity removal effect and high purity.
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[0035] 1. Preparation of chlorinated products of Gymast
[0036] Add 160g of 3-cyano-4-methoxy-2-(1H)pyridone and 1600ml of glacial acetic acid into a 2L reaction flask, raise the temperature to 42-45°C, start adding 112ml of sulfuryl chloride dropwise, take about 1.5h, keep warm React at 20°C for 6h, TLC monitors until the raw material is faint, distill the solvent under reduced pressure, concentrate the obtained solid and add 500ml of methanol, cool down to 10°C and stir for 0.5h, filter with suction, rinse with a little methanol. About 170g of the wet product is obtained, and the material is blown and dried at 60°C to obtain 155-160g of the chlorinated product, with a yield of 80-85%. HPLC greater than 99.0%.
[0037] 2. The preparation of the crude product of Gymast
[0038] Put the chlorinated product into a 2L reaction flask, add 800ml of 48% hydrobromic acid, heat up to 110°C and reflux for 24h. After the reaction was detected by TLC, 10% liquid caustic soda was adde...
Embodiment 1
[0042] Add 20 g of the crude product prepared above into 400 ml of 5% sodium hydroxide solution, stir to dissolve, add 2 g of activated carbon, then dropwise add 60 g of acetone, stir at room temperature for 3 h, filter the activated carbon, adjust the pH to 6.5 with 10% hydrochloric acid, stir at room temperature for 1 h, filter , washed the filter cake with a little acetone and purified water, and baked at 55-60°C for 8 hours in a vacuum to obtain 16.8g of the finished product of Jimostel. The appearance is off-white to white powder, and the product yield is 84.0%. figure 1 , see Table 1 for the contents of each component in the product. From the data analysis, it can be seen that the impurity content is extremely low. After calculation, the product purity is 99.98%, and the total impurity (that is, the total impurity) is less than 0.1%.
[0043]
Embodiment 2
[0045]Add 20 g of the crude product prepared above into 300 ml of 10% sodium hydroxide solution, stir to dissolve, add 2 g of activated carbon, then dropwise add 60 g of ethanol, stir at room temperature for 3 h, filter the activated carbon, adjust the pH to 7.0 with 10% hydrochloric acid, stir at room temperature for 1 h, filter , wash the filter cake with a little ethanol and purified water, and dry it in vacuum at 55-60°C for 8 hours to obtain 17.1g of Gemmost product, which is white powder in appearance and the product yield is 85.5%. The liquid phase spectrum is shown in figure 2 , the contents of each ingredient in the product are shown in Table 2. From the data analysis, it can be seen that the impurity content is extremely low. After calculation, the product purity is 99.99%, and the total impurity is less than 0.1%.
[0046]
PUM
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