s-3-cyclohexenecarboxylic acid and its purification method
A technology of cyclohexenecarboxylic acid and S-3-, which is applied in organic chemistry methods, separation/purification of carboxylic acid compounds, organic chemistry, etc., can solve the problem of inability to synthesize edoxaban, unsatisfactory purification purity, and many influencing parameters and other problems, to achieve the effect of facilitating large-scale industrial production, highlighting substantive characteristics, and simple refining methods
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Embodiment 1
[0023] The present embodiment provides a method for purifying S-3-cyclohexenecarboxylic acid, and the specific steps include:
[0024] Dissolve 1.26kg of crude S-3-cyclohexenecarboxylic acid and 1.28kg of R-a-phenethylamine in ethyl acetate, heat up to 70°C, stir and reflux for 1h, cool to 20°C after the reaction, filter and dry to obtain 2.32 kg of S-3-cyclohexenecarboxylic acid-R-a-phenethylamine salt. The crude S-3-cyclohexenecarboxylic acid refers to S-3-cyclohexenecarboxylic acid with an ee value of less than 97%.
[0025] Dissolve the S-3-cyclohexenecarboxylic acid-R-a-phenethylamine salt with ethanol at 80°C, cool down to 40°C for crystallization for 0.5h after dissolving, repeat the above operation 3 times after filtration; obtain recrystallized material ;
[0026] Add 3.7kg of methylene chloride, 5.5kg of water and the recrystallized material to the reaction vessel successively, add hydrochloric acid dropwise to maintain pH 2, stir at room temperature for 1h, collec...
Embodiment 2
[0031] The present embodiment provides a method for purifying S-3-cyclohexenecarboxylic acid, and the specific steps include:
[0032] According to the ratio of the molar ratio of S-3-cyclohexenecarboxylic acid crude product and R-a-phenethylamine to 1:1.5, the materials were weighed respectively, and then the weighed S-3-cyclohexenecarboxylic acid crude product and the weighed R-a- Phenethylamine was dissolved in ethyl acetate, heated to 90 °C, stirred and refluxed for 2 h, cooled to 30 °C after the reaction, filtered and dried to obtain S-3-cyclohexenecarboxylic acid-R-a-phenethylamine salt. The crude S-3-cyclohexenecarboxylic acid refers to S-3-cyclohexenecarboxylic acid with an ee value of less than 97%.
[0033] Dissolve the S-3-cyclohexenecarboxylic acid-R-a-phenethylamine salt with ethanol at 80°C, cool down to 40°C for crystallization for 0.5h after the dissolution, repeat the above operation 3 times after filtration; obtain recrystallized material ;
[0034] Add 4.6...
Embodiment 3
[0037] The present embodiment provides a method for purifying S-3-cyclohexenecarboxylic acid, and the specific steps include:
[0038] According to the ratio of the molar ratio of S-3-cyclohexenecarboxylic acid crude product and R-a-phenethylamine to 1:1, the materials were weighed respectively, and then the weighed S-3-cyclohexenecarboxylic acid crude product and the weighed R-a- Phenylethylamine was dissolved in ethyl acetate, heated to 70°C, stirred and refluxed for 2h, cooled to 25°C after the reaction, filtered and dried to obtain S-3-cyclohexenecarboxylic acid-R-a-phenethylamine salt;
[0039] Dissolve the S-3-cyclohexenecarboxylic acid-R-a-phenethylamine salt with ethanol at 85°C, cool down to 40°C for crystallization for 0.5h after dissolving, and repeat the above operation 3 times after filtration; obtain a recrystallized material ;
[0040]4.3kg of dichloromethane, 6.2kg of water and the recrystallized material were successively added to the reaction vessel, hydroch...
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