Preparation method of (1R) - (-) -10 Camphorsulfonic acid
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Preparation method of (1R) - (-) -10 Camphorsulfonic acid

Views: 9     Author: Site Editor     Publish Time: 2020-02-27      Origin: Site

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A method for inducing crystallization and splitting racemic camphor sulfonic acid to produce left and right camphor sulfonic acid, comprising the following steps:


(1) Preparation of racemic camphor sulfonate: add racemic substances and 1.2 times the weight of water to a stirring vessel, mix well, raise the temperature to 50-80 ℃, react for 1-3 hours, cool to 20-50 ℃, adjust the pH to 5-8 with ammonia water, keep it warm for 3-5 hours, cool to 5-15 ℃, and filter to obtain white racemic camphor sulfonate;


(2) Preparation of D-camphor sulfonate: Control the weight ratio of racemic camphor sulfonate, water, and D-optical activity inducer to be 1:1.2:0.1. Add racemic camphor sulfonate and water in proportion to a stirring vessel, heat up to 80-100 ℃, maintain for 1-2 hours, cool down to 50-60 ℃, add D-optical activity inducer in proportion, keep it warm for 1-3 hours, cool down to 20-40 ℃, and filter to obtain D-camphor sulfonate. The filtrate is used to prepare L-camphor sulfonate chemicalbook salt;


(3) Preparation of L-3-bromoacamphor-10-sulfonate: Add racemic camphor sulfonate to the filtrate in step (2), control the weight ratio of racemic camphor sulfonate to water: L-optical activity inducer to be 1:1.2:0.1, add racemic camphor sulfonate to water in proportion to the stirring vessel, add the stirring vessel, heat up to 80-100 ℃, maintain for 1-2 hours, cool down to 50-60 ℃, add the racemic optical activity inducer in proportion to the ratio, keep it warm for 1-3 hours, cool down to 20-40 ℃, filter to obtain L-camphor sulfonate, and use the filtrate to prepare D-optical activity inducer. Camphor sulfonate;


(4) Preparation of left and right camphor sulfonic acid: Dissolve the obtained left and right camphor sulfonic acid salts in water to prepare a 20% to 30% aqueous solution, and place them in two ion stirring columns. Collect the column solution and place it in an evaporator to evaporate to anhydrous. Then add acetic acid solvent, crystallize, cool to 5-20 ℃, and filter to obtain the product.


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