Synthetic preparation method of wintergreen oil
A technology of wintergreen oil and synthetic reaction, which is applied in the preparation of organic compounds, carboxylic acid ester preparation, chemical instruments and methods, etc., can solve the problems of complex catalyst preparation process, complex reaction follow-up treatment, complex synthetic reaction, etc., and shorten the production process. Effects of cycle, increasing difficulty, and simple reaction process
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Embodiment 1
[0022] Embodiment 1: use methyl formate as catalyst-small test to prepare wintergreen oil
[0023] According to the molar ratio of 2:1:0.2, accurately weigh 128.16g of methanol, 276.24g of salicylic acid, and 24.02g of methyl formate, and put them into the high-pressure reactor in turn, control the reaction temperature at 150°C, and the pressure at 0.9MPa. Under the reaction 6h. After the reaction is completed, the temperature is lowered to normal temperature, the reaction solution is transferred to a three-necked flask, and the 25 cm packed column (with ceramic Pall rings as the filler) is subjected to rough steaming under normal pressure to collect methanol fractions at 30-66°C. After the collection is completed, the vacuum pressure is controlled at -0.09 ~ -0.10MPa, and the fraction at 75-80°C is collected until no liquid evaporates. 298.45 g of finished wintergreen oil was obtained, the product purity was 99.6%, and the conversion rate was 97.78%.
Embodiment 2
[0024] Embodiment 2: make catalyzer-small test preparation wintergreen oil with methyl acetate:
[0025] Accurately weigh 128.16g of methanol, 276.24g of salicylic acid, and 29.63g of methyl acetate according to the molar ratio of 2:1:0.2, and put them into a high-pressure reactor in sequence. The reaction was stirred for 6h. After the reaction was completed, the temperature was lowered to normal temperature, the reaction solution was transferred to a three-necked flask, and the 25cm packed column (with ceramic Pall ring as the filler) was subjected to rough steaming under normal pressure to collect fractions at 50-66°C. After the collection is completed, the vacuum pressure is controlled at -0.09 ~ -0.10MPa, and the fraction at 75-80°C is collected until no liquid evaporates. Obtain 272.01g of finished wintergreen oil, product purity is 99.6%, conversion rate is 89.12%.
Embodiment 3
[0026] Embodiment 3: use methyl butyrate as catalyst-small test to prepare wintergreen oil:
[0027] Accurately weigh 128.16g of methanol, 276.24g of salicylic acid, and 40.85g of methyl butyrate according to the molar ratio of 2:1:0.2, and put them into a high-pressure reactor in sequence. Control the reaction temperature at 150°C and the pressure at 0.9MPa. The reaction was stirred for 6h. After the reaction was completed, the temperature was lowered to normal temperature, the reaction solution was transferred to a three-necked flask, and the 25 cm packed column (with glass Pall ring as the filler) was subjected to rough steaming under normal pressure to collect fractions at 50-66°C. After the collection is completed, the vacuum pressure is controlled at -0.09 ~ -0.10MPa, and the fraction at 75-80°C is collected until no liquid evaporates. Obtain 263.52g of finished wintergreen oil, the product purity is 99.5%, and conversion rate is 86.25%.
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