A kind of citral dibornyl acetal derivative and its preparation method and application
A technology of citral dimethyl acetal and citral, which is applied in the field of citral dibornyl acetal derivatives and its preparation, can solve the problems of strong volatility, low drug efficacy, poor solubility, etc., and achieve mild reaction conditions , the difficulty is not high, and the derivatives are stable
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Embodiment 1
[0058]Preparation of a citral dibornyl acetal derivative, such asfigure 1 As shown, including the following steps:
[0059](1) At room temperature, weigh 7.6120g (0.05mol, molecular weight of 152.23) of citral and 21.2240g (0.20mol, molecular weight of 106.12) of trimethyl orthoformate into a dry and clean round bottom flask and dissolve them in 50mL of methanol. 28.56mg p-toluenesulfonic acid was added, and the reaction system was refluxed for 6 hours at 80°C and 800r / min;
[0060](2) Add a saturated aqueous sodium bicarbonate solution to the reaction system in batches to pH=7-8, remove p-toluenesulfonic acid, concentrate under reduced pressure, extract 3 times with 30 mL dichloromethane, collect the organic layer, and add 9.4522 g anhydrous sulfuric acid Sodium removes water for 6 hours;
[0061](3) Filter to remove anhydrous sodium sulfate, remove the solvent under reduced pressure, use a silica gel column with an average particle size of 48μm for analysis: first dissolve the silica gel i...
Embodiment 2
[0071](1) At room temperature, weigh 3.8221 g (0.025 mol) of citral and 10.3421 g (0.097 mol) of trimethyl orthoformate in a dry and clean round bottom flask, dissolve in 40 mL of methanol, and add 15.21 mg of p-toluene sulfonate Acid, the reaction system is refluxed for 4 hours at 75°C and 800r / min.
[0072](2) Add a saturated aqueous sodium bicarbonate solution to the reaction system in batches to pH=7-8, remove the p-toluenesulfonic acid, concentrate under reduced pressure, extract 3 times with 30 mL of dichloromethane, collect the organic layer, and add 5.3214 g of anhydrous sulfuric acid Sodium removes water for 4 hours.
[0073](3) Filter to remove anhydrous sodium sulfate, remove the solvent under reduced pressure, use a silica gel column with an average particle size of 37μm for analysis, after loading the sample, first use 50mL of a slightly larger ratio (petroleum ether: ethyl acetate = volume ratio 15 :1) Wash with the eluent, flush out the impurities with small polarity, and t...
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