A new method for the synthesis of benzyl salicylate by solid-liquid phase transfer catalysis
A technology of benzyl salicylate, solid-liquid phase, applied in chemical instruments and methods, preparation of organic compounds, catalytic reactions, etc., can solve the problems of high cost and high cost of benzyl alcohol, and achieve low cost, reaction conversion rate and high efficiency. The effect of high selectivity and reduced difficulty
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Embodiment 1
[0024] A new method for the synthesis of benzyl salicylate by solid-liquid phase transfer catalysis: get sodium salicylate 84.05g (525mmol), benzyl chloride 63.3g (500mmol), crown ether (25mmol) and sodium iodide (3mmol), add three circles In a bottom flask, react at a temperature of 140°C for 3 hours. After the reaction is completed, add water to separate the layers of the reaction solution, separate the organic layer, wash the organic layer with distilled water, and then use 5% NaHCO 3 Wash twice with aqueous solution and twice with distilled water. Then dehydration and vacuum distillation are carried out, and the fraction at 164-165°C / 730Pa is collected to obtain the benzyl salicylate product. The product is a colorless transparent liquid, and it is a white needle crystal at low temperature. Gas chromatography is used for detection, the product purity is 99.37%, and the product yield is 92.72%. The conversion rate of benzyl chloride is 98.62%, and the reaction selectivity ...
Embodiment 2
[0026] A new method for the synthesis of benzyl salicylate by solid-liquid phase transfer catalysis: Take 96.1g (600mmol) of sodium salicylate, 63.3g (500mmol) of benzyl chloride, PEG-600 (25mmol) and potassium iodide (3mmol), add three round bottom In the flask, react at a temperature of 145°C for 4 hours. After the reaction is completed, add water to separate the layers of the reaction solution, separate the organic layer, wash the organic layer with distilled water, and then use 5% NaHCO 3 Wash twice with aqueous solution and twice with distilled water. Then dehydration and vacuum distillation are carried out, and the fraction at 164-165°C / 730Pa is collected to obtain the benzyl salicylate product. The product is a colorless transparent liquid, and it is a white needle crystal at low temperature. Gas chromatography is used for detection, the product purity is 99.78%, and the product yield is 95.27%. The conversion rate of benzyl chloride is 98.91%, and the reaction selecti...
Embodiment 3
[0028] A new method for the synthesis of benzyl salicylate by solid-liquid phase transfer catalysis: take 315.05g (1.97mol) of sodium salicylate, 237.98g (1.88mol) of benzyl chloride, PEG-2000 (94mmol) and potassium chloride (11.27mmol) , put it into a three-neck round bottom flask, and react at a temperature of 145°C for 4 hours. After the reaction is completed, add water to separate the layers of the reaction solution, separate the organic layer, wash the organic layer with distilled water, and then use 5% mass percent concentration of NaHCO 3 Wash twice with aqueous solution and twice with distilled water. Then dehydration and vacuum distillation are carried out, and the fraction at 164-165°C / 730Pa is collected to obtain the benzyl salicylate product. The product is a colorless transparent liquid, and it is a white needle crystal at low temperature. Gas chromatography is used for detection, the product purity is 99.40%, and the product yield is 94.13%. The conversion rate...
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