Monomer spice Mal-Phe for tobacco as well as preparation method and application of monomer spice
A technology of monomers and fragrances, which is applied in the field of preparation and new type of tobacco monomer fragrance Mal-Phe, to achieve the effect of increased yield, high yield and easy availability of raw materials
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Embodiment 1
[0028] A preparation method for tobacco monomer spice Mal-Phe, comprising the steps of:
[0029] Add 1 gram of maltose, 1.3 mL of dimethylformamide, and 3.0 mL of anhydrous methanol into a three-necked flask equipped with a thermometer and a condenser, reflux at 70°C for 23 minutes, then add 0.183 grams of phenylalanine and reflux for another 23 minutes. Finally, 0.032 g of strong acidic ion exchange resin and 0.176 g of myricetin were added for reflux reaction for 1 h; after the reaction, 0.339 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 6:2:1, 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...
Embodiment 2
[0031] A preparation method for tobacco monomer spice Mal-Phe, comprising the steps of:
[0032] Add 1 gram of maltose, 3.3 mL of dimethylformamide, and 1.9 mL of anhydrous methanol into a three-necked flask equipped with a thermometer and a condenser, reflux at 83°C for 29 minutes, then add 0.386 grams of phenylalanine and reflux for another 29 minutes. Finally, 0.049 g of strong acidic ion exchange resin and 0.562 g of myricetin were added for reflux reaction for 3.7 h; after the reaction, 0.97 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.
Embodiment 3
[0034] A preparation method for tobacco monomer spice Mal-Phe, comprising the steps of:
[0035] Add 1 gram of maltose, 3.6 mL of propylene glycol and 1.8 mL of anhydrous methanol into a three-necked flask with a thermometer and a condenser, reflux at 88°C for 46 minutes, then add 0.458 grams of phenylalanine and reflux for another 46 minutes, and finally add 0.061 grams of Strongly acidic ion exchange resin and 0.891 g of myricetin were refluxed for 7.5 hours; after the reaction, separated by silica gel column chromatography and recrystallized to obtain 0.671 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.
[0036] (1) Structural characterization of the target product
[0037] Through infrared spectroscopy (IR), high-resolution mass spectrometry (HR-MS), carbon nuclear magnetic resonance spectroscopy ( 13 C-NMR) carried out structural character...
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