Refinement method for ibuprofen
A refining method and organic solvent technology, applied in the field of chemical drug synthesis, can solve the problems of low purity and achieve the effects of improving purity, reducing pollution, and low cost
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Embodiment 1
[0060] Embodiment 1: the refining method of ibuprofen
[0061] 1. Refining method:
[0062] 1) Slowly add 1000g of ibuprofen coarse powder (content: 98.80%) to 5L of petroleum ether (60-90°C, which is a category of petroleum ether based on the boiling point), heat to 70°C, and stir to dissolve To homogeneous phase, after standing for 0.5h, cool down to room temperature naturally, place the reaction mixture at -5--1°C to crystallize for 1.5h, a white solid precipitates, filter, and use ice-bathed petroleum ether (60-90°C ) wash the solid, slowly suction filter (speed about 100ml / min), after drying, obtain the filter cake, and reclaim the filtrate;
[0063] 2) The filter cake is mixed with 5 L of petroleum ether (60-90° C.) for recrystallization again, and the operation of step 1) is repeated twice;
[0064] After three times of crystallization, the filter cake was vacuum-dried to obtain 458.8 g of high-purity ibuprofen refined product, with a yield of 45.88%.
[0065] 2. Det...
Embodiment 2
[0069] Embodiment 2: the refining method of ibuprofen
[0070] 1. Refining method:
[0071] 1) Slowly add 1000g (content: 98.80%) of ibuprofen oral raw material into 5L of n-heptane, heat to 70°C, stir and dissolve until homogeneous, after standing for 0.5h, cool naturally to room temperature, and react Put the mixture at -5--1°C, crystallize for 1.5h, and a white solid precipitates out, filter, wash the solid with ice-bathed n-heptane, and then slowly suction filter (speed about 100ml / min), drain and recover the filtrate .
[0072] 2) The filter cake is recrystallized after being mixed with 5 times (volume to weight ratio) of n-heptane again, and the operation of step 1) is repeated twice. After three times of crystallization, the filter cake was vacuum-dried to obtain 399.9 g of high-purity ibuprofen refined product, with a yield of 39.99%.
[0073] 2. Detection of ibuprofen purity:
[0074] The detection method is the same as in Example 1, and the final test results sho...
Embodiment 3
[0075] Embodiment 3: the refining method of ibuprofen
[0076] 1. Refining method:
[0077] 1) Slowly add 1000g of ibuprofen oral raw material (content: 98.80%) into 3L of petroleum ether (60-90°C), heat to 70°C, stir and dissolve until homogeneous, let stand for 0.5h, and cool naturally To room temperature, place the reaction mixture at -5--1°C to crystallize for 1.5h, a white solid precipitates out, filter, wash the solid with ice-bathed petroleum ether (60-90°C), and slowly suction filter (speed about 100ml / min), after draining, obtain filter cake, reclaim filtrate;
[0078] 2) The filter cake is mixed with 3 L of petroleum ether (60-90° C.) for recrystallization, and the operation of step 1) is repeated twice.
[0079] After three times of crystallization, the filter cake was vacuum-dried to obtain 408.6 g of high-purity ibuprofen refined product, with a yield of 40.86%.
[0080] 2. Detection of ibuprofen purity:
[0081] The detection method is the same as in Example...
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