Compound of Lansoprazole and a preparation method thereof
The technology of a kind of lansoprazole, compound is applied in the refined field of lansoprazole compound, can solve the problems such as the low purity of lansoprazole raw material, the purity of refined product has not obtained corresponding improvement, reaches easy operation, simple operation, Guarantee the effect of product quality
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Embodiment 1
[0027] Add 200 grams of crude product lansoprazole to dissolve in 1000ml ethanol, add 2mol / L sodium hydroxide solution 300ml to react, control final pH value to be 11.2, gained solution is eluted and purified with 400ml purified water after D1300 type macroporous adsorption resin, Collect the eluate, add 3.02 g of activated carbon to absorb for 30 minutes, filter, add 4 mol / L sodium dihydrogen phosphate solution to the filtrate, precipitate crystals, control the final pH value of the reaction solution to 7.6, filter, wash the crystals with 400 ml of purified water, 40 °C Drying under reduced pressure for 5 hours yielded 188.8 grams of lansoprazole refined product, with a yield of 94.4% and a purity of 99.8%.
Embodiment 2
[0029] 200 grams of crude product lansoprazole is added to react in 600ml of 1mol / L sodium hydroxide solution, and the control final pH value is 11.1, and the gained solution is eluted and purified with 300ml purified water after the BS-55 type macroporous adsorption resin, collects and washes Remove the liquid, add 1.88 g of activated carbon to absorb for 30 minutes, filter, add 2 mol / L sodium bicarbonate solution to the filtrate, precipitate crystals, control the final pH value of the reaction solution to 7.8, filter, wash the crystals with 300 ml of purified water, and dry under reduced pressure at 45 °C 4 hours, 182.6 grams of delansoprazole refined product, the yield is 91.3%, and the purity is 99.9%.
Embodiment 3
[0031] Add 200 grams of crude product lansoprazole to dissolve in 900ml of methanol, add 400ml of 1.5mol / L potassium hydroxide solution to react, and control the final pH to be 11.0, and the resulting solution is washed with 500ml of purified water after the BS-55 type macroporous adsorption resin Depurify, collect the eluate, add 3.34 grams of activated carbon to absorb for 30 minutes, filter, add 2mol / L sodium bisulfate solution to the filtrate, precipitate crystals, control the final pH value of the reaction solution to 7.7, filter, wash the crystals with 500ml purified water, Drying under reduced pressure at 45°C for 8 hours yielded 184.2 grams of refined lansoprazole, with a yield of 92.1% and a purity of 99.9%.
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