Advanced intermediate of rosuvastatin calcium and preparation method of advanced intermediate
A technology for rosuvastatin calcium and advanced intermediates, which is applied in the field of synthesis of drugs and drug intermediates, and can solve problems such as unfavorable industrial application and promotion, difficulty in balancing production cost and product quality, and high cost
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[0056] Example 1
[0057] Feed 120g D4 (95~105g after 100% reduction), 100g sodium carbonate, 60g 2-mercapto-5-ethyl-1,3,4-thiadiazole and 250g DMAC, turn on stirring and heat up to 100~110°C, and keep the temperature for 8 hours. The temperature was lowered to below 100°C, and concentrated under reduced pressure until there was no fraction. Cool down, add 550 g of dichloromethane and 400 g of drinking water, stir evenly, and then let stand for stratification. The organic layer is D4-1 solution.
[0058] The D4-1 solution was transferred to the reactor, 150g of drinking water, 5g of sodium carbonate and 3g of tetrabutylammonium chloride were fed, stirred and dissolved, and the temperature was controlled at 10-15°C. Add dropwise a mixture of 450g 50% hydrogen peroxide and 6g ammonium tungstate, and control the temperature to 15~20℃. Keep stirring for 20 hours. After the reaction was completed, the reaction solution was left to stand for stratification, and the organic layer...
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[0059] Example 2
[0060] Feeding 110gD4 (87~97g after 100%), 110g sodium bicarbonate, 50g 2-mercapto-5-methyl-1,3,4-thiadiazole and 225gDMF, open stirring and be warming up to 110~120 ℃ after, be incubated for 7 Hour. The temperature was lowered to below 100°C, and concentrated under reduced pressure until there was no fraction. Cool down, add 500 g of dichloromethane, 425 g of drinking water, stir evenly, and let stand for stratification. The organic layer is D4-1 solution.
[0061] The D4-1 solution was transferred to the reactor, 130 g of drinking water, 8 g of sodium bicarbonate and 2.2 g of tetrabutylammonium bromide were fed, stirred and dissolved, and the temperature was controlled at 15 to 20 °C. A mixture of 500g 30% hydrogen peroxide and 5g ammonium molybdate was added dropwise, and the temperature was controlled at 20-25°C. Keep stirring for 16 hours. After completion of the reaction, the reaction solution was left to stand for stratification, and the organic ...
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[0062] Example 3
[0063] Feeding 130gD4 (100~110g after 100%), 90g potassium carbonate, 70g 2-mercapto-5-phenyl-1,3,4-thiadiazole and 260g tert-butyl alcohol, after opening and stirring and being warming up to 90~100 ℃, Keep warm for 10 hours. The temperature was lowered to below 85°C, and concentrated under reduced pressure until there was no fraction. Cool down, add 615 g of dichloromethane, 400 g of drinking water, stir evenly, and let stand for stratification. The organic layer is D4-1 solution.
[0064] The D4-1 solution was transferred to the reactor, 160 g of drinking water, 6.5 g of potassium bicarbonate and 4 g of dodecyl trimethyl ammonium chloride were fed, stirred and dissolved, and the temperature was controlled at 20 to 25 °C. A mixture of 835g of 30% hydrogen peroxide and 6g of ammonium phosphomolybdate was added dropwise, and the temperature was controlled at 25-30°C. Keep stirring for 22 hours. After completion of the reaction, the reaction solution was ...
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