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With toluene-4-sulfonic acid; hydroquinone; In diethylene glycol dimethyl ether; at 140℃; for 10h;Inert atmosphere;
152 g (1.05 mol) of <strong>[51792-34-8]3,4-dimethoxythiophene</strong>, 775 g (8.42 mol) of glycerin, 19.9 g (0.105 mol) of p-toluenesulfonic acid monohydrate, 11.5 g (0.105 mol ) of Hydroquinone and 3.68 L of diglyme were added to a reactor, and then the inside of the reaction system was sufficiently purged with argon gas. The oxygen concentration in the reaction vessel gas atmosphere was 0.3 vol percent. Thereafter, the mixture was heated to 140 ° C and stirred for 10 hours. After cooling to room temperature, the reaction solution was analyzed by gas chromatography and the formation rate of the target product (2) was 75percent and the formation rate of the by-product (4) was 0.5percent (molar ratio 99.3 : 0.7). 1.68 L of a 10percent sodium hydroxide aqueous solution was added and the mixture was allowed to stand for 12 hours. The solvent was distilled off and extracted three times with a toluene / saturated aqueous sodium chloride solution. The toluene layer was concentrated and dried and dissolved in 3.7 L of a mixed solvent of toluene / ethyl acetate = 4/1, and the insoluble matter was filtered off. The solvent was distilled off and dissolved in 220 g of toluene, then 220 g of hexane was further added, and the mixture was allowed to stand at about 10 ° C for 2 hours. The obtained crystals were filtered, then washed with hexane and dried under vacuum to obtain 100 g of the desired product (2) as a white precipitate (yield: 55percent). By gas chromatography, 0.5percent of the by-product (4) was contaminated, and the purity of the target product (2) was 99.5percent.
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