Phenoxy aromatic acid with cyclopropyl and pharmaceutically acceptable salt thereof as well as preparation method and application thereof
A phenoxyaromatic acid and pharmacy technology, applied in the field of medicine, can solve problems such as insufficient medicinal effect, and achieve the effects of improving stability and improving medicinal effect
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[0050] The preparation of comparative example fenofibric acid and choline salt thereof
[0051] (1) Preparation of fenofibric acid
[0052] Add 72.0 g of fenofibrate and 360 ml of absolute ethanol into a 500 ml reaction bottle, stir and mix. Raise the temperature to 60°C, heat and stir until the solid dissolves into a colorless transparent solution, add 57.6g of 25% sodium hydroxide solution dropwise, and keep the temperature at about 60°C during the dropwise addition. End; the temperature of the reaction solution is lowered to 0-5°C, add concentrated hydrochloric acid dropwise to adjust the pH value of the reaction solution to 2-3, after the drop is complete, stir at 0-5°C for 30 minutes, filter, wash the filter cake with pure water until neutral, and drain , and dried at 65°C to obtain 60.1 g of fenofibric acid.
[0053] (2) Preparation of choline fenofibric acid
[0054] Dissolve 10.0 g of fenofibric acid in 100 ml of isopropanol and heat to 65°C. The choline hydroxide / ...
Embodiment 1
[0055] The preparation of embodiment 1 cyprofenofibric acid
[0056]
[0057] Add 11.2g of anhydrous aluminum trichloride, 42.4ml of toluene, and 7.9ml of anisole into the three-neck flask, stir, control the temperature below 40°C, and slowly add 7.36ml of 4-chlorobenzoyl chloride dropwise. After the dropwise addition, The oil bath was slowly heated to reflux, and reacted for 2 hours. The reaction was tracked by TLC. After the reaction was complete, it was cooled to room temperature, and 50 ml of water was slowly added dropwise under stirring. At this time, a large amount of solids were precipitated, filtered with suction, and the filter cake was washed with an appropriate amount of water. The resulting solids were recrystallized with ethanol to obtain 10.8 g of compound (II).
[0058]
[0059] Add 8.0g of the compound (II) prepared in the previous step, 0.6g of sodium hydroxide, and 96ml of butanone into the three-neck flask, heat up to 45-60°C with stirring, stir for 3...
Embodiment 2
[0061] The preparation of embodiment 2 cycloprofen norofibric acid choline salt
[0062]
[0063] Add 7.5g of ciprofenofibric acid, 75ml of isopropanol, and 6.26g of choline hydroxide solution (45wt%) into the reaction flask. It was heated to 65°C and stirred for 1 hour, then naturally cooled to room temperature, and a solid precipitated out. The solid was collected and dried to give 6.88 g of ciprofen norficate choline salt. m / z: 418.14 (100.0%), 420.14 (32.0%), 419.15 (24.3%), 421.14 (7.8%), 420.15 (3.8%); Elemental Analysis: C, 63.08; H, 6.02; Cl, 8.46; N , 3.34; O, 19.10.
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