A kind of synthetic preparation method of wintergreen oil
A technology for wintergreen oil and synthesis reaction, which is applied in the preparation of organic compounds, preparation of carboxylic acid esters, chemical instruments and methods, etc., can solve the problems of complex catalyst preparation process, complex post-reaction treatment, complex synthesis reaction, etc., and shorten the production time. The effect of cycle, easy purification, and simple reaction process
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Embodiment 1
[0022] Example 1: Catalyst as methylene carboxylate - small test preparation of winter boiled oil
[0023] According to the ratio of molar ratio 2: 1: 0.2, 128.16 g of methanol, 276.24 g of salicylic acid, 24.02 g of formate, sequentially put into high pressure reactor, control the reaction temperature 150 ° C, pressure 0.9 MPa, in agitation The reaction was at 6 h. After the reaction was completed, the reaction solution was transferred to the normal temperature, and the 25 cm filler column (the Bauer ring of the ceramic material) was crude, and the methanol fraction of 30-66 ° C was collected. After the collection is completed, the vacuum pressure is controlled at -0.09 ~ -0.10 MPa, and the fraction of 75-80 ° C is collected until there is no liquid steamed. 298.45 g of finished winter oil was obtained, with a purity of 99.6%, and the conversion rate was 97.78%.
Embodiment 2
[0024] Example 2: Catalyst as a methyl acetate - small test prepared for winter oil:
[0025] According to the ratio of molar ratio 2: 1: 0.2, 128.16 g of methanol, 276.24 g of salicylic acid, methyl acetate 29.63 g, sequentially put into the high pressure reactor, control the reaction temperature at 150 ° C, pressure at 0.9 MPa, The reaction was reacted for 6 h. After the reaction was completed, the reaction solution was transferred to the three-necked flask, and the 25 cm filler column (in the filler of the ceramic material) was crude, and the fraction of 50-66 ° C was collected. After the collection is completed, the vacuum pressure is controlled at -0.09 ~ -0.10MPa, and the fraction of 75-80 ° C is collected, and until there is no liquid steamed. 272.01 g of finished winter oil was obtained, and the product purity was 99.6%, the conversion rate was 89.12%.
Embodiment 3
[0026] Example 3: Catalyst as methyl butyrorate - Try prepared winter oil:
[0027] According to the ratio of molar ratio 2: 1: 0.2, 128.16 g of methyl alcohol was accurately weighed, 276.24 g of salicylic acid was 20.85 g of butyrate, and the high pressure reactor was sequentially put into the high pressure reactor, the reaction temperature was 150 ° C, the pressure was 0.9 MPa, The reaction was reacted at a stirred state. After the reaction was completed, the reaction mixture was transferred to the normal temperature, and the 25 cm filler column (the Bauer ring of the glass material was carried out in normal pressure, and the fraction of 50-66 ° C was collected. After the collection is completed, the vacuum pressure is controlled at -0.09 ~ -0.10 MPa, and the fraction of 75-80 ° C is collected until there is no liquid steamed. 263.52 g of finished winter oil was obtained, and the purity of the product was 99.5%, the conversion rate was 86.25%.
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