Method for synthesizing sodium 2-carboxyphenylborate
A technology of sodium carboxyphenyl borate and methoxycarbonyl phenyl borate, which is applied in the field of synthesizing sodium 2-carboxyphenyl borate, can solve the problems of long steps, cumbersome operation, unsuitability for the preparation process of sodium 2-carboxyphenyl borate, etc., and achieve cost Low cost, easy to obtain raw materials, and easy operation
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Embodiment 1
[0018] 2- Under the protection of nitrogen, put 280g THF, 43g methyl 2-bromobenzoate and trimethyl borate (1.5eq is the molar ratio) into a 500mL four-necked bottle, cool down to -85~-75℃, add Butyllithium n-hexane solution 60g1.1eq, after dripping, keep stirring for 2 hours, sample 10% hydrochloric acid to quench, and HPLC detects that the raw material is less than 6.5%. Stir naturally to raise the temperature to -20~15°C, add 99g of 10% hydrochloric acid aqueous solution dropwise to quench the reaction, the quenching process will release heat, the system temperature should be controlled below 0~5°C, pH=4~5, the system is stratified , separate the tetrahydrofuran layer and concentrate under reduced pressure, the water layer is extracted with 80 g of ethyl acetate each time, and the extraction is total 2 times, the ethyl acetate layer and the concentrated tetrahydrofuran layer are combined, washed once with 15-20 g of sodium chloride aqueous solution, and the organic phase is ...
Embodiment 2
[0021] The first step is the same as in Example 1
[0022] Add 29.5g of 2-methoxycarbonylphenylboronic acid and 60g of methanol into a 250mL reactor, and add 26.2g of 25% sodium hydroxide dropwise at a temperature of 45-50°C. After the dropwise addition, keep warm at 45-50°C for 2 hours, and check whether there are any raw materials left in the reaction solution in LC, and add sodium hydroxide if there is any. There is no remaining raw material for post-processing, vacuum distillation to no liquid, the obtained solid is added to the mother liquor acetone + new acetone for the first beating, a total of 60g, the temperature is raised to 50°C for beating, and then the temperature is gradually lowered to 0°C for beating for 0.5h, and the solid is obtained by filtration. Dry, a total of 32g, yield 95%, lc99.8%.
Embodiment 3
[0024] 3- Under nitrogen protection, put 280g THF, 43g methyl 2-bromobenzoate and 49g (1.28eq) triisopropyl borate into a 500mL four-necked bottle, cool down to -85~-75℃, add n-butyl Lithium-based n-hexane solution 60g1.1eq, after dripping, keep stirring for 2 hours, sample 10% hydrochloric acid to quench, and HPLC detects that the raw material is less than 1.6%. Naturally raise the temperature and stir to raise the temperature to -20~15°C, add dropwise 99g of 10% hydrochloric acid aqueous solution to quench the reaction, the quenching process will release heat, the system temperature should be controlled below 0~5°C, pH=4~5, the system will be layered, The tetrahydrofuran layer was separated and concentrated under reduced pressure, the water layer was extracted with 80 g of ethyl acetate each time, a total of 2 extractions, the ethyl acetate layer and the concentrated tetrahydrofuran layer were combined, washed once with 15-20 g of aqueous sodium chloride solution, and the org...
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