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A technology of intermediates and reaction solvents, applied in the field of organic chemical synthesis, can solve problems such as excessive waste, flammability of active nickel, and complicated post-treatment
Inactive Publication Date: 2021-07-20
SHENZHEN HUAXIAN PHARMA TECH CO LTD
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Problems solved by technology
[0014] Step 2: The post-treatment is complicated, and a lot of acid is used to adjust the pH, and there are a lot of three wastes
[0015] Step 3: Post-processing extraction and concentration takes a long time;
[0016] Step 4: Active nickel is very flammable, and the safety risk is very large
Method used
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Embodiment 1
[0049] (1) Synthesis of AMLF02
[0050]
[0051] Add p-fluoronitrobenzene (50kg), DMSO (190.25kg), diethyl methylmalonate (70.4kg) into the reaction kettle, start stirring, add anhydrous powder potassium carbonate (73kg), and heat up to 70-80 °C, react for 15-17 hours. Cool down to 20-30°C, and add dropwise 30% sodium hydroxide solution (432kg) at a temperature of 20-50°C. After dropping, heat to 50-60°C for 1-2 hours. After standing for 1 h, the lower high saline phase was separated. Cool down to 20-30°C, add water (350kg), and adjust pH to 7-8 with concentrated hydrochloric acid. Dichloromethane (390 kg) was added to extract impurities twice. Control the temperature at 20-30°C and use concentrated hydrochloric acid to pH 2-3, add dichloromethane (455kg) and extract once. The organic phase was washed once by adding water (300kg), and concentrated to dryness under reduced pressure to obtain 128.6kg of AMLF02 with a crude product purity of 98.92%. The above-mentioned w...
Embodiment 2
[0056] (1) Synthesis of AMLF02
[0057]
[0058] Add p-fluoronitrobenzene (50kg), DMF (190.25kg), diethyl methylmalonate (70.4kg) into the reaction kettle, start stirring, add anhydrous sodium carbonate (56kg), and heat up to 70-80°C , react for 15-16 h. After the reaction is finished, the temperature is lowered to 20-30° C., and 30% potassium hydroxide solution (432 kg) is added dropwise at 20-50° C. under temperature control. After dropping, heat to 50-60°C and react for 1-2h. After standing for 1 h, the lower high saline phase was separated. Cool down to 20-30°C, add water (350kg), and adjust pH to 7-8 with concentrated hydrochloric acid. Impurities were extracted twice by adding ethyl acetate (390 kg). Control the temperature at 20-30°C and use concentrated hydrochloric acid to pH 2-3, add ethyl acetate (455kg) and extract once. The organic phase was washed once by adding water (300 kg), concentrated to dryness under reduced pressure to obtain 127.5 kg of AMLF02, a...
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Abstract
The invention discloses a preparation method of an alminoprofen intermediate, belongs to the field of organic chemical synthesis, and provides a new technical route for improving the defects of synthetic reaction of ethyl 2-(4-amino-phenyl)propionate: 1) taking p-fluoronitrobenzene and diethyl methylmalonate as raw materials, adding alkali, conducting heating, finishing the reaction, conducting cooling, conducting hydrolyzing with alkali, after the reaction is finished, conducting layering, conducting washing with water, extracting impurities, adjusting the pH value, extracting a product, and conducting concentrating to obtain AMLF02; 2) heating AMLF02 in a solvent to 55-75 DEG C, and dropwise adding thionyl chloride for esterification reaction, conducting cooling, adjusting the pH, directly adding a catalyst for reduction at the temperature of 70-80 DEG C, after the reaction is finished, conducting filtering with the aid of diatomite, neutralizing the filtrate to 7-8, conducting concentrating to remove ethanol, extracting a water phase with methylbenzene, and conducting concentrating to obtain AMLF04. The method has the beneficial effects that the problem of slow filtration is solved, extraction is omitted, time is saved, and cost is saved; direct layering is performed after reaction, the amount of hydrochloric acid is reduced, and the treatment difficulty of three wastes is reduced; and safe hydrazine hydrate replaces active nickel.
Description
technical field [0001] The invention belongs to the field of organic chemical synthesis, and in particular relates to a preparation method of an alminprofen intermediate. Background technique [0002] Aminoprofen is a non-steroidal anti-inflammatory analgesic drug, which is an aromatic phenylpropionic acid derivative. It exerts anti-inflammatory, analgesic and detumescence effects by inhibiting cyclooxygenase, bradykinin and phosphatase A2. Its curative effect is equal to or better than indomethacin, ibuprofen, etc. It is suitable for rheumatism and rheumatoid arthritis, nerve root pain, tendonitis, trauma (fracture, contusion, sprain), dysmenorrhea, and postpartum uterine colic , toothache, otitis media, etc. In addition, because of its strong anti-penetration ability, it can prevent and treat acute joint cavity effusion. [0003] [0004] Ethyl 2-(4-amino-phenyl)propionate is an important intermediate in the synthesis of alminoprofen and has broad market prospects. ...
Claims
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