Synthesis method of glabridin
A technology of glabridin and a synthetic method, applied in directions such as organic chemistry, can solve problems such as long cycle, and achieve the effects of high total yield, fast and efficient synthesis, and short total route
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[0025] 1. Add 0.30g (1.85mmol) of 7-hydroxycoumarin into a 10mL round bottom flask, add 3mL of acetonitrile, 0.31mL (2.04mmol) of DBU and 0.32mg (0.00185mmol) of copper chloride dihydrate in turn, at 0°C Slowly add 0.22mL (1.94mmol) of 2-methyl-3-butyn-1-ol, react at room temperature for 10h, and TLC monitors that the reaction of raw materials is complete. Pour the reaction solution into saturated NaHCO 3 In aqueous solution, after extraction with ethyl acetate, over anhydrous MgSO 4 Dry, filter, concentrate under reduced pressure, and separate by column chromatography (eluent: EA / PE=1:3) to obtain compound I (0.37g, yield 90%, white solid, Mp: 253-255°C), reaction equation As follows:
[0026]
[0027] The structural characterization data of the obtained compound I are: 1 H NMR (400MHz, CDCl 3 )δ7.64(d, J=9.2Hz, 1H), 7.36(d, J=8.8Hz, 1H), 7.32(d, J=2.0Hz, 1H), 7.04(dd, J=8.4, 2.0Hz, 1H), 6.28(d, J=9.6Hz, 1H), 2.66(s, 1H), 1.71(s, 6H); HRMS(ESI) m / z: theoretical value ...
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