A kind of Mogrosin A derivative and its preparation method and application
A technology of AHA and derivatives, which is applied in the preservation, application, and food science of food ingredients as antimicrobials, and can solve problems such as unknown active ingredients.
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Embodiment 1
[0036] (S1) get 4.72g (0.01mol) of mogrosin acid methyl, 4g ethyl acetate and petroleum ether mixed solvent (v / v=1:1), 0.05g anhydrous DMF is put into reaction vessel, drip slowly under 50 ℃ of stirring conditions 3.57g of thionyl chloride (0.03mol) was added, and the dropwise addition was completed within 1h, and the reaction was kept at 50°C for 5h. During the reaction, the tail gas was absorbed by 10% NaOH aqueous solution, and the excess thionyl chloride and solvent were evaporated after the reaction;
[0037] (S2) slowly add the mixed solution of 1.61g sodium hydroxymethanesulfonate (0.012mol) and 5g anhydrous DMF to (S1) reaction vessel, complete dropwise addition within 1h, control system temperature to react at 40 ℃ for 12h, the reaction After the end, adjust the pH to 9-9.5 with saturated NaHCO3, stand for stratification, take the organic layer, add 3 g of anhydrous sodium sulfate, stand for 3 hours to remove the water in the solvent, filter, evaporate the solvent, use...
Embodiment 2
[0040] Other operations and conditions are the same as in Example 1, except that in step (S2) 1.61 g of sodium isethionate is replaced with 1.78 g of sodium isethionate (0.012 mol). Finally, 5.23 g of white crystals were obtained, the HPLC purity was 99.0%, and the yield was 86.0%. It is a compound in which n=2 in the structure of formula (I), which is compound 2.
[0041] 1 HNMR (CDCl 3 ): 0.76 (3H, s, C28), 0.93 (3H, d, C21), 1.18 (3H, d, C29), 1.22 (3H, s, C18), 1.38 (1H, m, C20), 1.45 (1H , d, C8), 1.56 (2H, m, C2), 1.61 (1H, t, C17), 1.85 (3H, s, C26), 2.13 (1H, d, C10), 2.52 (1H, d, C12- H a ), 2.62 (1H, d, C4), 2.70 (1H, d, C12-H b ), 3.24 (2H, t), 3.55 (1H, d, C19-H a ), 3.81 (1H, t, C3), 4.18 (2H, t), 4.65 (1H, d, C19-H b ), 6.87 (1H, t, C24). ESI: MS(M-Na): 551.3.
Embodiment 3
[0043] Other operations and conditions are the same as in Example 1, except that in step (S2) 1.61 g of sodium hydroxymethanesulfonate is replaced by 2.11 g of sodium 4-hydroxybutanesulfonate (0.012 mol). Finally, 5.49 g of white crystals were obtained, the HPLC purity was 99.1%, and the yield was 86.3%. It is the compound of formula (I) where n=4, which is compound 3.
[0044] 1 HNMR (CDCl 3 ): 0.76 (3H, s, C28), 0.93 (3H, d, C21), 1.18 (3H, d, C29), 1.22 (3H, s, C18), 1.38 (1H, m, C20), 1.45 (1H , d, C8), 1.61 (1H, t, C17), 1.85 (3H, s, C26), 2.13 (1H, d, C10), 2.52 (1H, d, C12-H a ), 2.62 (1H, d, C4), 2.70 (1H, d, C12-H b ), 3.26 (2H, t), 3.55 (1H, d, C19-H a ), 3.81 (1H, t, C3), 4.02 (2H, t), 4.65 (1H, d, C19-H b ), 6.87 (1H, t, C24). -O-CH on huangbutyl 2 -CH 2 -CH 2 -CH 2 -SO 3 The H on the two methylene groups in the middle of Na is mixed with the H on the other methylene groups in the mogro acid A, and cannot be distinguished. ESI: MS(M-Na): 579.3.
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