Refining process of crude product for preparing high-quality imidazole aldehyde
A technology for high-quality imidazolaldehyde and crude product is applied in the field of crude product refining technology for preparing high-quality imidazolaldehyde, can solve the problems of dark color, difficult to meet the requirements of pharmaceutical intermediates, yellowish appearance of finished products, etc. Effect
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Embodiment 1
[0024] 1) Dissolve 100 g of imidazole aldehyde crude product (imidazole aldehyde content 84.32%) in 400 mL of water, adjust the pH to 12.5, raise the temperature to 50-55 ° C, add 2 g of activated carbon, stir for 1 hour and filter to obtain filtrate A;
[0025] 2) Add 150 mL of chloroform to the filtrate A, stir and wash, separate layers, take out the water layer, adjust the pH to 6-7, cool and filter to obtain the filtrate;
[0026] 3) Add the filtrate to a mixed solvent of 150g of isopropanol and 150g of water, stir and raise the temperature to 50-55°C, add 1g of activated carbon after it dissolves, stir for 1 hour, and then filter to obtain filtrate B;
[0027] 4) Add 400mL of water dropwise to filtrate B at 50-55°C, stir and cool down to 0-5°C after dripping, crystallize, and dry to obtain 70.98g of imidazolaldehyde finished product (purity 99.99%, total yield 84.17%).
Embodiment 2
[0029] 1) Dissolve 100 g of imidazole aldehyde crude product (imidazole aldehyde content 79.48%) in 400 mL of water, adjust the pH to 12.5, heat up to 50-55 °C, add 3 g of activated carbon, stir for 1 hour and filter to obtain filtrate A;
[0030] 2) Add 150 mL of methyl chloride to the filtrate A, stir and wash, separate layers, take out the water layer, adjust the pH to 6-7, cool down and filter to obtain the filtrate;
[0031] 3) Add the filtrate to a mixed solvent of 150L n-propanol and 150L water, stir to raise the temperature to 50-55°C, add 2g of activated carbon after it dissolves, stir for 1 hour and then filter to obtain filtrate B;
[0032] 4) Add 400mL of water dropwise to filtrate B at a temperature of 50-55°C, stir and cool down to 0-5°C after dripping, crystallize, and dry to obtain 80.7g of imidazolaldehyde finished product (purity 99.99%, total yield 95.72%).
Embodiment 3
[0034] 1) Dissolve 100 g of imidazole aldehyde crude product (imidazole aldehyde content 82.78%) in 400 mL of water, adjust the pH to 12.5, raise the temperature to 50-55 ° C, add 2 g of activated carbon, stir for 1 hour and filter to obtain filtrate A;
[0035] 2) Add 150 mL of dichloromethane to the filtrate A, stir and wash, separate layers, take out the water layer, adjust the pH to 6-7, cool down and filter to obtain the filtrate;
[0036] 3) Add the filtrate to a mixed solvent of 150L methanol and 150L water, stir to raise the temperature to 50-55°C, add 2g of activated carbon after it dissolves, and filter after stirring for 1 hour to obtain filtrate B;
[0037] 4) Add 400mL of water dropwise to filtrate B at a temperature of 50-55°C, stir and cool down to 0-5°C after dripping, crystallize, and dry to obtain 65.22g of imidazolaldehyde finished product (purity 99.99%, total yield 78.80%).
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