The refining method of valsartan
A refining method and valsartan technology, applied in the field of chemical refining, can solve problems such as being difficult to remove, and achieve the effect of easy operation
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Embodiment 1
[0023] Put 20g of crude valsartan and 150ml of ethyl acetate into a reaction bottle, heat up to 45-55°C, add 15g of 200-300 mesh neutral alumina after the solid is fully dissolved, keep stirring at 45-55°C for 4 hours, filter, filter The cake was washed with a small amount of ethyl acetate, drained, and the filtrates were combined.
[0024] Transfer the washing filtrate into a reaction bottle, stir at 30-35°C until solids are precipitated, continue to stir for 2 hours, then slowly add 90ml of n-hexane dropwise, then cool down to about 20°C and stir for 2 hours, filter with suction, and use the filter cake Appropriate amount of ethyl acetate: n-hexane = 1:1 (volume ratio) mixed solution was washed, drained, and dried under reduced pressure to obtain 17.8 g of solid. The HPLC purity of valsartan was 99.81%, and the impurity content of butyryl valsartan is 0.12%, and the impurity content of propionyl valsartan is 0.03%.
Embodiment 2
[0026] Put 20g of crude valsartan and 150ml of ethyl acetate into a reaction bottle, raise the temperature to 45-55°C, add 15g of 200-300 mesh acidic alumina after the solid is fully dissolved, keep stirring at 45-55°C for 4 hours, filter, and filter cake Wash with a small amount of ethyl acetate, drain, and combine the filtrates.
[0027] Transfer the washing filtrate into a reaction bottle, stir at 30-35°C until solids are precipitated, continue to stir for 2 hours, then slowly add 90ml of n-hexane dropwise, then cool down to about 20°C and stir for 2 hours, filter with suction, and use the filter cake Appropriate amount of ethyl acetate: n-hexane = 1:1 (volume ratio) mixed solution was washed, drained, and dried under reduced pressure to obtain 18.0 g of solid. The HPLC purity of valsartan was 99.79%, and the impurity content of butyryl valsartan was 99.79%. is 0.12%, and the impurity content of propionyl valsartan is 0.04%.
Embodiment 3
[0029] Put 20g of crude valsartan and 200ml of ethyl acetate into the reaction bottle, raise the temperature to 45-50°C, add 15g of 200-300 mesh neutral alumina after the solid is completely dissolved, keep stirring at 45-50°C for 4 hours, filter, filter The cake was washed with a small amount of ethyl acetate, drained, and the filtrates were combined.
[0030] Transfer the washing filtrate into a reaction bottle, add 120ml of n-hexane, stir evenly, let it stand and slowly cool to room temperature, then put it in the refrigerator overnight, filter it with suction, and use an appropriate amount of ethyl acetate:n-hexane=1:1 ( The mixed solution of volume ratio) was washed, drained, and dried under reduced pressure to obtain solid 17.5g, the HPLC purity of valsartan was 99.82%, the impurity content of butyryl valsartan was 0.11%, and the impurity content of propionyl valsartan was 0.03%.
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