Method for preparing high-purity losartan
A losartan, high-purity technology, applied in the field of preparation of high-purity losartan, can solve the problems of no practical production significance, no competitiveness, complicated process, etc., and achieve the effect of low cost, environmental friendliness and high refining yield
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[0019] The first step: add 200ml of toluene, 45g of biphenyl bromide, 30g of imidazole aldehyde, and 0.5g of tetrabutylammonium bromide in sequence; add sodium hydroxide aqueous solution to react at room temperature until the raw materials have reacted completely, layer and wash. The organic layer is reduced by adding a reducing agent, crystallized by adding water, filtered, and dried to obtain the compound represented by formula 1.
[0020] Step 2: Add 150ml of toluene in sequence; add 43g of the compound shown in formula 1, catalyst, 30g of sodium azide, the reaction, the reaction is over, the product is extracted with sodium hydroxide aqueous solution, sodium nitrite, ethyl acetate are added dropwise hydrochloric acid to pH To 3-5, filter and wash the filter cake with water to obtain crude losartan to be refined (purity 95%-98%).
Embodiment 1
[0022] Add 50g of the crude losartan obtained by the above route into a 250ml three-necked flask, add 150ml of methanol; then heat to 60°C, stir for 1 hour, cool to 3°C, stir and crystallize for 2 hours, filter, and dry to obtain high purity Losartan , The yield is 90%, the purity is 99.4%, and the single impurities are 0.2%.
Embodiment 2
[0024] Add 50g of the crude losartan obtained by the above route into a 250ml three-necked flask, add 150ml of acetone; then heat to 60°C, stir for 1 hour, cool to 3°C, stir and crystallize for 2 hours, filter and dry to obtain high purity Losartan , The yield is 94%, the purity is 99.5%, and the single impurities are 0.15%.
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