A kind of preparation method of landylol oxalate
A compound and weight technology, applied in the preparation of an important intermediate product of landiolol hydrochloride, the field of preparation technology of landiolol oxalate, can solve the problem of difficult to use pharmaceutical injection preparations, unfavorable industrialized production, low product yield, etc. problem, to avoid alcoholysis, low cost, simple operation effect
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Embodiment 1
[0030] Embodiment 1, the preparation of compound I
[0031] Add 1565.5g of compound III and 3000g of water into the reaction flask, stir and heat up to t 内 =45°C, dissolve clear, use 1190g of 40% sodium hydroxide (475g of sodium hydroxide dissolved in 715g of water) to adjust the pH to 10-11, control the temperature below 50°C, a large amount of yellow solid precipitates, cool down to 30-35°C in an ice bath , add 500g of compound II, 3000g of N,N-dimethylformamide, and keep it warm at 30-35°C for 3-4 hours. After TLC confirms that the reaction of compound II is complete, filter it, extract the filtrate with 800mL×3 isopropyl ether, and collect the water layer , extracted with 3000 mL×4 ethyl acetate, combined the organic layers, and washed with 5000 mL×3 saturated brine. Collect the organic layer, add 2000g of anhydrous sodium sulfate and 100g of activated carbon, stir and dry for 2-3 hours to decolorize. Filtrate, evaporate the filtrate to dryness under reduced pressure a...
Embodiment 2
[0032] Embodiment 2, the preparation of compound I
[0033] Add 1956.9g of compound III and 5000g of water into the reaction flask, stir and heat up to t 内=45°C, dissolve clear, use 1313g of 40% sodium hydroxide (525g of sodium hydroxide dissolved in 788g of water) to adjust the pH to 10-11, control the temperature below 50°C, a large amount of yellow solids are precipitated, cool down to 40-45°C in an ice bath , add 500g of compound II, 5000g of dimethyl sulfoxide, and incubate at 40-45°C for 3-4h. After TLC confirms that the reaction of compound II is complete, filter and extract the filtrate with 800mL×3 isopropyl ether, collect the aqueous layer, and wash with 3000mL×4 Extract with ethyl acetate, combine the organic layers, and wash with 5000 mL×3 saturated brine. Collect the organic layer, add 2000g of anhydrous sodium sulfate and 100g of activated carbon, stir and dry for 2-3 hours to decolorize. Filtrate, evaporate the filtrate to dryness under reduced pressure at 6...
Embodiment 3
[0034] Embodiment 3, the preparation of compound I
[0035] Add 1174.2g of compound III and 1500g of water into the reaction flask, stir and heat up to t 内 =45°C, dissolve clear, use 40% sodium hydroxide 1063g (425g sodium hydroxide dissolved in 638g water) to adjust the pH to 10-11, control the temperature below 50°C, a large amount of yellow solid precipitates, at 45-50°C, add the compound Ⅱ 500g, N,N-dimethylacetamide 1500g, keep warm at 45~50℃ for 3~4h, TLC confirms that the reaction of compound Ⅱ is complete, filter, the filtrate is extracted with 800mL×3 isopropyl ether, collect the water layer, and use 3000mL ×4 extracted with ethyl acetate, the combined organic layers were washed with 5000 mL×3 saturated brine. Collect the organic layer, add 2000g of anhydrous sodium sulfate and 100g of activated carbon, stir and dry for 2-3 hours to decolorize. Filtrate, evaporate the filtrate to dryness at 60°C under reduced pressure, add 6.5kg of absolute ethanol to the residue,...
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