Gingerol compounds and their use as flavor modifiers
A kind of technology of compound and mixture, applied in the field of gingerol compounds
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Embodiment 1
[0243] The separation of embodiment 1.[6]-gingerol, [8]-gingerol or [10]-gingerol
[0244] A plant extract containing [6]-gingerol as a main component such as ginger extract (Layn-CN nominal 75%, NMR: 55%) was dissolved in methanol, followed by washing 3 times with cyclohexane to obtain the product. The product was purified on a RP-18 silica gel column (GraceReveleris, H 2 O / ACN 50:50) on flash chromatography to obtain [6]-gingerol (α D +23.2° (c=1, CHCl 3 )), [8]-gingerol (α D +15.1° (c=1, CHCl 3 )) or [10]-gingerol (α D +16° (c=1, CHCl 3 )).
Embodiment 2
[0245] The synthesis of embodiment 2.[6]-gingerdiol
[0246] Diethyl(methoxy)borane (2.1 mL; 15.98 mmol) was added to [6]-gingerol (4.0 g, 13.32 mmol) in 120 mL THF / MeOH (4:1) at -78 °C in the solution. The reaction mixture was stirred at -78 °C for 30 min, then NaBH was added 4 (0.605 g; 15.98 mmol). The reaction mixture was stirred at -78°C for 3 hours, and 30% H 2 o 2 (48 mL), a mixture of phosphate buffer (pH=7; 96 mL) and MeOH (methanol, 96 mL). Evaporate the solvent and wash with CH 2 Cl 2 The remaining aqueous phase was extracted twice. The combined organic phases were washed with water. use Na 2 SO 4 Dry and evaporate. The residue was treated with 8.0 mL of glacial acetic acid (acetic acid) in 120 mL of EtOAc (ethyl acetate) at room temperature to complete the decomposition of the diol borate. The mixture was stirred at room temperature for 2 h and washed with 40 mL of saturated NaHCO 3 Quenched. Then, it was extracted 2 times with EtOAc. The combined ...
Embodiment 3
[0247] Embodiment 3.[6]-Synthesis of Gingeriol Diacetate
[0248] Triethylamine (5.56g, 4 equivalents), acetic anhydride (4.91g, 3.5 equivalents) and 4-dimethylaminopyridine (DMAP, 67mg, 0.3 equivalents) were continuously added to [6]-gingerdiol (4.2g, 13.7mmol) in a solution in 120mL. The reaction mixture was stirred overnight and worked up. The product was purified by flash chromatography (heptane:EtOAc, 6:4) to yield 3.6 g (61%) of [6]-gingertriacetate. A solution of [6]-ginger triacetate (2.4 g, 5.7 mmol) in pyrrolidine (24 ml) was stirred at room temperature for 1.5 hours. After work-up and flash chromatography (heptane:EtOAc, 6:4), 1.49 g (69%) of [6]-gingeriol diacetate was obtained as off-white oil (α D -1.2° (c=1, CHCl 3 )).
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