Preparation method of 3-hydroxyl-4-methoxycinnamaldehyde
A technology of methoxycinnamaldehyde and hydroxyl group, which is applied in the field of preparing 3-hydroxy-4-methoxycinnamaldehyde, can solve the problems of many reaction by-products, low preparation efficiency, low product yield and the like, and achieves product yield Improves, shortens the reaction time, increases the effect of the activity
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Embodiment 1
[0012] Dissolve 1.008g (0.015mol) of potassium hydroxide in 100ml of aqueous methanol (volume ratio of methanol to water: 1:1), then add 15.2g (0.1mol) of isovanillin and 0.456g of polytetrahydrofuran (the number average molecular weight is 250) , stir well to make it evenly mixed. After cooling to -5°C, 35.36 g (0.225 mol) of acetaldehyde aqueous solution with a mass fraction of 28% was continuously added dropwise to the reaction system to start the reaction, and the dropping process continued for 5 hours. After the dropwise addition, the stirring reaction was continued for 2 h, and then 1.9 ml of hydrochloric acid with a mass fraction of 36% was added for neutralization to end the reaction. After suction filtration, a light yellow crystal was obtained, which was the crude product of 3-hydroxy-4-methoxycinnamaldehyde. Add the crystals into 300ml of methanol, stir for 2h, filter with suction, and wash the filter cake with 50ml of methanol. The resulting filter cake was added...
Embodiment 2
[0014] Dissolve 0.56g (0.010mol) of potassium hydroxide in 100ml of aqueous methanol (volume ratio of methanol to water: 1:1), then add 15.2g (0.1mol) of isovanillin and 0.304g of polytetrahydrofuran (the number average molecular weight is 650) , stir well to make it evenly mixed. After cooling to 0° C., 35.36 g (0.225 mol) of acetaldehyde aqueous solution with a mass fraction of 28% was continuously added dropwise to the reaction system to start the reaction, and the dropping process continued for 4 hours. After the dropwise addition, the stirring reaction was continued for 1 h, and then 1.1 ml of hydrochloric acid with a mass fraction of 36% was added for neutralization to end the reaction. After suction filtration, a light yellow crystal was obtained, which was the crude product of 3-hydroxy-4-methoxycinnamaldehyde. Add the crystals into 300ml of methanol, stir for 2h, filter with suction, and wash the filter cake with 50ml of methanol. The resulting filter cake was added...
Embodiment 3
[0016] Dissolve 0.336g (0.006mol) of potassium hydroxide in 100ml of aqueous methanol (volume ratio of methanol to water: 1:1), then add 15.2g (0.1mol) of isovanillin and 0.304g of polytetrahydrofuran (the number average molecular weight is 1000) , stir well to make it evenly mixed. After cooling to 10° C., 19.64 g (0.125 mol) of acetaldehyde aqueous solution with a mass fraction of 28% was continuously added dropwise to the reaction system to start the reaction, and the dropping process continued for 3 hours. After the dropwise addition, the stirring reaction was continued for 1 h, and then 0.65 ml of hydrochloric acid with a mass fraction of 36% was added for neutralization to end the reaction. After suction filtration, a light yellow crystal was obtained, which was the crude product of 3-hydroxy-4-methoxycinnamaldehyde. Add the crystals into 300ml of methanol, stir for 2h, filter with suction, and wash the filter cake with 50ml of methanol. The resulting filter cake was a...
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