Novel securinine dimer as well as preparation method and application thereof
A technology of hagiline dimer and dimer, which is applied in the field of medicine, can solve the problems affecting the treatment effect, achieve the effect of improving cognitive function, optimizing the activity of inducing neural differentiation and promoting protein synthesis, and good stability
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Embodiment 1
[0057] The general preparation method of embodiment 1 compound N1~N6
[0058]
[0059] At room temperature, dissolve chinensis (217mg, 1mmol) in a stirred mixed solvent of dichloromethane (5mL) and methanol (0.5mL), and add potassium phosphate (K 3 PO 4 , 64mg, 0.3mmol) and the corresponding primary amine (R-NH 2 ,5mmol). After heating up to 35°C, the reaction was carried out for 8 hours. The organic solvent was concentrated under reduced pressure to obtain a crude product. The obtained crude product was separated and purified by silica gel column chromatography to obtain the corresponding compounds N1-N6.
Embodiment 2
[0060] The preparation of embodiment 2 compound 1
[0061]
[0062] At room temperature, dissolve trimethylsilyl azide (6.58mL, 50mmol) and acetic acid (2.86mL, 50mmol) in a stirred dichloromethane (50mL) solvent at room temperature. and DBU (75L, 0.5mol). After the temperature was raised to 35°C, the reaction was carried out for 8 hours, and the organic solvent was concentrated under reduced pressure to obtain a crude product. The obtained crude product was separated and purified by silica gel column chromatography to obtain a pair of diastereomer azides N10a and N10b. Subsequently, the azide compound N10a was dissolved in a stirred DMSO (2 mL) solvent, and copper (127 mg, 2 mmol), copper sulfate pentahydrate (13 mg, 0.05 mmol) and 1,5-hexadiyne (26 μL, 0.27 mmol) were successively added ). After reacting in the dark for 5 hours, ethyl acetate (10 mL) was added, and the filtrate was obtained by filtration. The filtrate was washed 3 times with water (3×10 mL), washed wi...
Embodiment 3
[0064] The preparation of embodiment 3 compound 2
[0065]
[0066] Referring to the synthesis method of Example 2, using the azide compound N10b as the starting material, a white solid compound 2 was obtained (47% yield).
[0067] 1H NMR (300MHz, CDCl3) δ7.30(d, J=10.2Hz, 2H), 5.78(d, J=22.4Hz, 2H), 4.81(s, 2H), 3.58(s, 2H), 3.38(s ,4H),3.03(s,9H),2.43(dd,J=11.1,5.7Hz,2H),1.86(s,2H),1.70–1.13(m,13H); 13CNMR(75MHz,CDCl3)δ172.3,171.1 , 146.9, 120.4, 111.5, 90.4, 64.1, 60.1, 48.7, 32.3, 28.1, 25.9, 25.0, 23.9, 21.7; HR-ESI-MS m / z 599.3088 [M+H]+.
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