Method for preparing D, L-pantolactone through normal-pressure reduction
A technology of pantotolactone and pantoacid, which is applied in the field of preparation of D,L-pantotolactone, can solve problems such as high-risk processes and potential safety hazards, and achieve easy production operations, low production costs, and simple processes Effect
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[0027] Example 1
[0028] Add 74g (0.5mol) of 50% glyoxylic acid to a 500ml three-necked flask, cool the cooling device to 15℃, slowly add 53.12g (0.525mol) of triethylamine, add triethylamine, stir at 25℃ After 30 minutes, add 39.6g (0.55mol) of isobutyraldehyde, increase the temperature to 70°C and react for 6 hours, then lower the temperature to 15°C, slowly add 27g (0.5mol) potassium borohydride, after the addition is complete, react for 4 hours, and slowly add Add 70% sulfuric acid until the pH of the material liquid is 1.25, heat up to 87°C and react for 4 hours, cool the temperature to 15°C with the cooling device, adjust the pH of the material liquid to 7.5 with ammonia water, extract with dichloroethane, 300ml each time, combine the organic layers, The solvent was recovered by distillation, and under reduced pressure distillation was used to obtain 64 g of D,L-pantoate lactone, with a product yield of 98.5% and a purity of 99.16%.
Example Embodiment
[0029] Example 2
[0030] Add 92.5g (0.5 mole) of 40% glyoxylic acid to a 500ml three-necked flask, cool the cooling device to 25°C, slowly add 52.95g (0.725 mole) of diethylamine, after the addition of diethylamine, stir at 22°C After reacting for 30 minutes, 41.4g (0.575 mol) of isobutyraldehyde was added in flow, and the temperature was raised to 75°C to react for 7 hours, and the temperature was lowered to 20°C. 38g (1 mole) of sodium borohydride was slowly added. Add 80% sulfuric acid until the pH of the material liquid is 1.0, raise the temperature to 80°C and react for 3.5 hours, cool the temperature to 25°C with the cooling device, adjust the pH of the material liquid to 7.2 with sodium carbonate solution, extract with ethyl acetate, 280ml each time, combine the organic Layers, the solvent is recovered by distillation, and 63.5 g of D,L-pantoic acid lactone is obtained by distillation under reduced pressure. The product yield is 97.69% and the purity is 99.07%.
Example Embodiment
[0031] Example 3
[0032] Add 88.8g (0.6 mol) of 50% glyoxylic acid into a 500ml three-necked flask, cool the cooling device to 15°C, slowly add 30.54g (0.3 mol) of ethanolamine, after the addition of ethanolamine, stir and react at 30°C for 30 minutes. Add 43.2g (0.6 mol) of isobutyraldehyde, increase the temperature to 55°C and react for 7 hours, then lower the temperature to 15°C, slowly add 16.2g (0.3 mole) of potassium borohydride, after the addition is complete, react for 4 hours, slowly add 70% Sulfuric acid until the pH of the feed solution is 2, heated to 75°C for 4 hours, cooled to 15°C by the cooling device, adjusted the pH of the feed solution to 8 with ammonia water, extracted with ethyl acetate, 300ml each time, combined the organic layers, and distilled to recover the solvent. Under reduced pressure distillation, 76.44 g of D,L-pantoic acid lactone was obtained, the product yield was 98.0%, and the purity was 99.23%.
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