Monomer flavor Mal-Ile used for cigarettes as well as preparation method and application thereof
A technology of monomers and fragrances, applied in the field of preparation and new type of tobacco monomer fragrance Mal-Ile, achieving significant industrial application value and popularization and application, excellent physical moisturizing effect, and high yield effect
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Embodiment 1
[0028] A preparation method for tobacco monomer spice Mal-Ile, comprising the steps of:
[0029] Add 1 gram of maltose, 1.5 mL of dimethylformamide, and 2.8 mL of anhydrous methanol into a three-neck flask equipped with a thermometer and a condenser, reflux at 76°C for 20 minutes, then add 0.138 grams of isoleucine and reflux for another 20 minutes. Finally, 0.035 g of strong acidic ion exchange resin and 0.249 g of kaempferol were added for reflux reaction for 2.0 h; after the reaction, 0.395 g of the target product in the form of white crystals was obtained by silica gel column chromatography and recrystallization. Among them, the eluent used for column chromatography separation is a mixed solution composed of n-butanol, glacial acetic acid and water, the volume ratio of the three is 6:1:1, and the chromogenic agent is ninhydrin ethanol solution; the solvent used for recrystallization It is a mixed solution of absolute ethanol and absolute methanol with a volume ratio of 1:1...
Embodiment 2
[0031] A preparation method for tobacco monomer spice Mal-Ile, comprising the steps of:
[0032] Add 1 gram of maltose, 3.6 mL of dimethylformamide, and 2.0 mL of anhydrous methanol into a three-necked flask equipped with a thermometer and a condenser, reflux at 85°C for 35 minutes, then add 0.256 grams of isoleucine and reflux for another 35 minutes. Finally, 0.053 g of strong acidic ion exchange resin and 1.019 g of kaempferol were added for reflux reaction for 6.0 h; after the reaction, 0.845 g of the target product in the form of white crystals was obtained by silica gel column chromatography and recrystallization. Wherein, the operation process of column chromatography separation and recrystallization is the same as that of Example 1.
[0033]
Embodiment 3
[0035] A preparation method for tobacco monomer spice Mal-Ile, comprising the steps of:
[0036] Add 1 gram of maltose, 3.9 mL of propylene glycol and 1.7 mL of anhydrous methanol into a three-necked flask with a thermometer and a condenser tube, reflux at 89°C for 45 minutes, then add 0.396 grams of isoleucine and reflux for another 45 minutes, and finally add 0.068 grams of Strongly acidic ion exchange resin and 1.245 g of kaempferol were refluxed for 8.0 h; after the reaction, separated by silica gel column chromatography and recrystallized to obtain 0.584 g of the target product in the form of white crystals. Wherein, the operation process of column chromatography separation and recrystallization is the same as that of Example 1.
[0037] (1) Structural characterization of the target product
[0038] Through infrared spectroscopy (IR), high-resolution mass spectrometry (HR-MS), carbon nuclear magnetic resonance spectroscopy ( 13 C-NMR) carried out the structural charac...
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