Synthetic method of 2-thiophenylbenzoic acid
A technology of phenylthiobenzoic acid and a synthesis method, applied in the directions of sulfide preparation, organic chemistry, etc., can solve the problems of limited application of palladium catalytic system, expensive phosphorus ligand, expensive palladium catalyst, etc., and achieves easy realization of industrialized production, catalysis Good effect, less toxic effect
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Embodiment 1
[0037] Embodiment 1 (2: 1, sodium hydroxide, copper sulfate, DL-proline)
[0038] Add 0.35mmol (0.0539g) of thiosalicylic acid and 0.70mmol (0.0853g) of phenylboronic acid into the reaction tube, add 0.25mL of sodium hydroxide solution (10%), 0.05mL of anhydrous ethylenediamine, and then add 0.025mL of copper sulfate mmol (0.0040g) and DL-proline 0.025mmol (0.0029g) were used as catalysts, heated to 130°C for reaction, TLC tracking detection, the reaction was complete in 24 hours, TLC tracking determined that the reactant thiosalicylic acid disappeared, and then naturally After cooling to room temperature, the mother liquor was extracted with 170 ml of ethyl acetate, the organic layer was dried over anhydrous magnesium sulfate, and the solvent was evaporated to dryness to obtain a solid. First pass through the column with petroleum ether with a boiling range of 60-90°C, load the crude product, then pass through the column with petroleum ether with a boiling range of 60-90°C, a...
Embodiment 2
[0039] Embodiment 2 (2: 1, sodium hydroxide, copper sulfate, DL-alanine)
[0040]Add 0.35mmol (0.0539g) of thiosalicylic acid and 0.70mmol (0.0853g) of phenylboronic acid into the reaction tube, add 0.25mL of sodium hydroxide solution (10%), 0.05mL of anhydrous ethylenediamine, and then add 0.025mmol of copper sulfate (0.0040g) and DL-alanine 0.025mmol (0.0022g) as a catalyst, heated to 130 ° C for reaction, TLC tracking detection, the reaction was complete in 24 hours, TLC tracking determined that the reactant thiosalicylic acid disappeared, and then cooled naturally After reaching room temperature, the mother liquor was extracted with 170 ml of ethyl acetate, the organic layer was dried over anhydrous magnesium sulfate, and the solvent was evaporated to dryness to obtain a solid. First pass through the column with petroleum ether with a boiling range of 60-90°C, load the crude product, then pass through the column with petroleum ether with a boiling range of 60-90°C, and the...
Embodiment 3
[0041] Embodiment 3 (2: 1, sodium hydroxide, copper sulfate, 8-hydroxyquinoline)
[0042] Add 0.35mmol (0.0539g) of thiosalicylic acid and 0.70mmol (0.0853g) of phenylboronic acid into the reaction tube, add 0.25mL of sodium hydroxide solution (10%), 0.05mL of anhydrous ethylenediamine, and then add 0.025mmol of copper sulfate (0.0040g) and 0.025mmol (0.0036g) of 8-hydroxyquinoline as a catalyst, heated to 130 ° C for reaction, TLC tracking detection, the reaction was complete in 24 hours, TLC tracking determined that the reactant thiosalicylic acid disappeared, and then cooled naturally After reaching room temperature, the mother liquor was extracted with 170 ml of ethyl acetate, the organic layer was dried over anhydrous magnesium sulfate, and the solvent was evaporated to dryness to obtain a solid. First pass through the column with petroleum ether with a boiling range of 60-90°C, load the crude product, then pass through the column with petroleum ether with a boiling range...
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