A kind of preparation method of potassium guaiacol sulfonate
A technology of potassium guaiacol sulfonate and sulfonation reaction, applied in the field of medicine and chemical industry, can solve problems such as great difficulty, the invention patent technology has not been reported, and achieves simple post-processing, cheap and easy-to-obtain reaction raw materials, and reaction conditions. mild effect
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Embodiment 1
[0024] In a 500 ml three-necked flask, add 15.1 grams (0.1 moles) of 2-hydroxyacetanilide, 150 milliliters of dioxane, and 9.6 grams (0.12 moles) of sulfur trioxide, react at 80 ° C, and track the reaction with thin layer chromatography The raw material disappears, then add 20% (mass) dilute hydrochloric acid, the amount of dilute hydrochloric acid is based on 0.3 mole of hydrogen chloride, slowly add 100 ml of aqueous solution containing 20.7 g (0.3 mole) of sodium nitrite, and control the reaction temperature not to exceed 5 °C, use starch-potassium iodide test paper to check the status of free nitrous acid until the end of the reaction. Then slowly add the prepared diazonium salt solution dropwise into 100 ml of methanol solution containing 8 grams of potassium hydroxide, react at 100°C for 10 hours, add 10 grams of solid potassium chloride, stir to dissolve, and slowly cool , filtered, and dried to obtain 15.7 g of the product, with a yield of 65% and a purity of ≥99%.
Embodiment 2
[0026] In a 500 ml three-necked flask, add 15.1 grams (0.1 moles) of 2-hydroxyacetanilide, 75 milliliters each of dioxane and tetrachloroethane, and 12 grams (0.15 moles) of sulfur trioxide, and react at 90 ° C. Follow the disappearance of the reaction raw materials with thin-layer chromatography, then add 20% (mass) dilute hydrochloric acid, the amount of dilute hydrochloric acid is based on 0.5 moles of hydrogen chloride contained therein, slowly add 100 milliliters of aqueous solution containing 35 grams (0.5 moles) of sodium nitrite, Control the reaction temperature not to exceed 5°C, check the status of free nitrous acid with starch-potassium iodide test paper until the end of the reaction. Then slowly add the prepared diazonium salt solution dropwise into 100 ml of methanol solution containing 8 grams of potassium hydroxide, react at 100°C for 5 hours, add 10 grams of solid potassium chloride, stir to dissolve, and slowly cool , filtered, and dried to obtain 15 grams of ...
Embodiment 3
[0028] In a 500 ml three-necked flask, add 15.1 grams (0.1 moles) of 2-hydroxyacetanilide, 150 milliliters of tetrachloroethane, and 9.6 grams (0.12 moles) of sulfur trioxide, react at 60 ° C, follow the reaction with thin layer chromatography The raw material disappears, then add 20% (mass) dilute hydrochloric acid, the amount of dilute hydrochloric acid is based on 0.3 mole of hydrogen chloride, slowly add 100 ml of aqueous solution containing 20.7 g (0.3 mole) of sodium nitrite, and control the reaction temperature not to exceed 5 °C, use starch-potassium iodide test paper to check the status of free nitrous acid until the end of the reaction. Then slowly add the prepared diazonium salt solution dropwise into 100 ml of methanol solution containing 8 grams of potassium hydroxide, react at 100°C for 5 hours, add 10 grams of solid potassium chloride, stir to dissolve, and slowly cool , filtered, and dried to obtain 15.3 g of the product, with a yield of 63% and a purity of ≥99...
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